Ethanol → Ethyl 1-phenylindole-3-glyoxylate

HRID 863544

반응식

HRID 863544 반응식
[C:1]1([N:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[CH:9]=[CH:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:16](Cl)(=[O:20])[C:17](Cl)=[O:18].[CH2:22]([OH:24])[CH3:23]>C(OCC)C>[C:1]1([N:7]2[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9]([C:16](=[O:20])[C:17]([O:24][CH2:22][CH3:23])=[O:18])=[CH:8]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

5

반응물 3

HCID 702EthanolHCID 65578Oxalyl chlorideHCID 1820291-Phenyl-1H-indole

생성물 1

HCID 54522388Ethyl 1-phenylindole-3-glyoxylate

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

An ice-cooled solution of 10 g (51.8 mmol) of 1-phenylindole in 100 ml of anhydrous diethyl ether was treated dropwise during 5 minutes with a solution of 6 ml (68.8 mmol) of oxalyl chloride in 20 ml of anhydrous diethyl ether. The mixture was stirred for 3 hours while cooling with ice and then treated with 25 ml of ethanol in one portion. After stirring for 10 minutes, the solvent was removed under reduced pressure and the residual solid was crystallized from 60 ml of ethanol to give 12.38 g of ethyl 1-phenylindole-3-glyoxylate as a pale yellow solid of melting point 109°-110° C.

후처리

  1. temperaturewhile cooling with ice
  2. stirringAfter stirring for 10 minutes
  3. customthe solvent was removed under reduced pressure
  4. customthe residual solid was crystallized from 60 ml of ethanol

출처 및 근거

ORD 기록
ord-74de5377f25a4801900574f2bd9a1c83
출처 데이터셋
uspto-grants-1998_02
특허 번호
US05721230

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