Lab Report 3-Synthesis of Fluorescein PDF

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Name: Just i nPenn

LabSect i on:

Wed/Thu/Fr i

Poi nt s Awar ded

EXPERI MENT: Synt hesi sofFl uor escei n

Poi nt s Poss i bl e

I nt r oduct i on

5

React i onScheme/Mechani s m /Si deReact i on( s)

30

Exper i ment alPr ocedur e

15

Cal cul at i ons

5

Concl usi ons

5

Deduct i ons( t i me,saf et y ,l abk eepi ng) Subt ot al Techni queGr ade

40 TOTAL

Comment s :

60

100

I NTRODUCTI ON Fl uor es c ei ni safl uor es c entdy ec ommonl yus edi nfl uor es centmi c r os copyt oobs er v ec el ls t r uc t ur eand t hei rc omponent s .Themai nobj ec t i v ei nt hi sex per i mentwast os y nt hes i z efl uor esc ei nus i ngr es or c i nol ,pht hal i c anhy dr i de,andz i ncc hl or i de.Wewer eus i ngmet hodst hatweus edi npr ev i ousl abss uc hast her efl ux i ngoft he mat er i alandt hefi l t er i ngoft hes ol i dus i ngv ac uum fil t r at i ont oac hi ev et hepur es tc ompoundpos s i bl e.The i mpor t anceoft hi sex per i menti st ounder s t andt hec hemi c alpr oper t i esofdi ffer entcompoundsandhow per f or mi ngt her efl ux i ngandfi l t r at i onwi l l beabl et os epar at et hecompoundsi nt ot hedes i r edc omponent s .

REACTI ONSCHEME/MECHANI SM /SI DEREACTI ON( S)

EXPERI MENTALPROCEDURE Combi ne1. 00gRes or c i nol ,0. 60gpht hal i canhy dr i de,and1. 01gz i nc( I I )c hl or i dei nt oa50ml r ound bot t om fl as kandst i rt hor oughl y .Sett hes andbat ht o9andpl ac et hefl askequi ppedwi t hacondens eri nt ot he s andbat hs ot hatt hes ol i dmi x t ur ei sbel owt hel ev eloft hes and.Af t erami nut e ,t hemi x t ur ebegi nst omel tand c hangef r om awhi t ec ol ort oar eddi s h/ br ownc ol or .Keept hemi x t ur ei nt hes andbat hf oranaddi t i onal28 mi nut es ,l ower i ngt het emper at ur es et t i ngt o6t omak es ur et hatt hec ol oroft hemi x t ur edoesnott ur nbl ac k .Rai s e t hefl as kf r om t hes andbat h,l ett hemi x t ur ecoolf or6mi nut esands c r apet hes ol i dunt i ly ouhav es omes mal l pi ec esbr eakoff.Add15mlofdi s t i l l edwat erandaboi l i ngc hi p,andpl ac ebac ki nt ot hes andbat hata t emper at ur es et t i ngof4.Refl uxt hemi x t ur ef or30mi nut esandnot i cet hatt hec ol ort ur nsay el l owi s hhue.Af t er30 mi nut es ,l ett hemi x t ur ecoolf or5mi nut esandv ac uum fi l t ert her eact i onmi x t ur ef or5mi nut es .Di s connec tt he v ac uum andr i ns et hes ol i dwi t h3mlofwat er ,f ol l owedby3ml ofcol det hanol ,andt henv ac uum fi l t ert hemi x t ur e f oranot her15mi nut es .Rec or dt hewei ghtoft her eds ol i d( 2. 02g)andmeas ur et hemel t i ngpoi nt( 310318C) . T r ans f ermos tofy ourmi x t ur ei nt oat es tt ube,c or ki t ,andl abel i tus i ngt hei ns t r uct i onsf r om Lab1.Tak eas mal l amountoft hepr oductandpl acei ti nas mal lt es tt ube,add3ml ofwat erands hak et hemi x t ur e,not i c i ngt he s ol ut i onbec omesac l oudyr eddi s hc ol or .Pl ac et het es tt ubeundert heUVl ampandnot i c et hatt hemi xt ur edoes

notl i ghtup.Thenadd3dr opsof1M NaOHs ol ut i on,s hak et het es tt ube,andpl acei tundert heUVl amp,and not i c et hatt hes ol ut i onl i ght supafl uor es centgr eenc ol or .

CALCULATI ONS React ant s :1. 00gRes or c i nol ,0. 60gpht hal i canhy dr i de,Zi nc( I I )c hl or i dei sanac i dc at al y s tanddoesnotr eac t Mol armas s es :110. 1g/ molRes or c i nol ,148. 1g/ molpht hal i canhy dr i de Mol esofr eac t ant s :

g∗1 mol =0.009 mol Resorcinol 110.1 g g∗1 mol =0.004 mol Phthalic anhydride 0.60 148.1 g 1.00

Pr oduc t s :2. 02gFl uor es c ei n Mol armas s es :332. 3g/ mol Mol esofpr oduc t s :

2.02

g∗1mol =0.006 mol Fluorescein 332.2 g

Per centYi el d:

0.006 mol =0.4615∗100=46.2 % 0.009mol +0.004 mol

Mel t i ngpoi ntofFl uor es c ei n:310318C

CONCLUSI ONS Thi sl abwasnotv er ydi ffic ul tt oc ompl et ei fonef ol l owedt hedi r ect i onsandi twasal s onotv er yt i me c ons umi ngasIwasabl et ol eav ewel lbef or et heendoft hes c hedul edc l as s .Formyr es ul t s ,my46. 2% y i el dmay nots eem l i k eIac qui r edmuc hpr oduc tandt hati spr obabl ybec aus eal otoft hefl uor es c ei nwass t i l ls t uc kt omy fl as k ,andIwasnotabl et ogetal l ofi toutoft hegl as s war e.Howev er ,wi t hmymel t i ngpoi ntr angeof310318C, andt hel i t er at ur edat aof314C,i ts howst hatmyr es ul twaspur eandal mos tent i r el yfl uor es c ei n.Al s o,when pl ac edunderfl uor es c entl i ght ,t hepr oduc twasafl uor es centgr eenc ol orwhi c hdemons t r at est hatt hepr oductwas fl uor es cei n....