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Benzene → 2-Ethyl-2-phenyl-5-methoxy-6,7-dichloro-1-indanone

HRID 2052038
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HRID 2052038 반응식
C[O-].[Na+].[C:4]1([CH:10]2[CH2:18][C:17]3[C:12](=[C:13]([Cl:22])[C:14]([Cl:21])=[C:15]([O:19][CH3:20])[CH:16]=3)[C:11]2=[O:23])[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.I[CH2:25][CH3:26].C1C=CC=CC=1>O.CN(C)C=O>[CH2:25]([C:10]1([C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH2:18][C:17]2[C:12](=[C:13]([Cl:22])[C:14]([Cl:21])=[C:15]([O:19][CH3:20])[CH:16]=2)[C:11]1=[O:23])[CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 241BenzeneHCID 6340IodoethaneHCID 10942334Sodium MethoxideHCID 109904442-Phenyl-5-methoxy-6,7-dichloro-1-indanone

생성물 1

HCID 124235892-Ethyl-2-phenyl-5-methoxy-6,7-dichloro-1-indanone

시약·촉매·용매 2

HCID 962Water용매
HCID 6228
Dimethylformamide
용매

실험 절차

Sodium methoxide (1.24 g., 0.023 mole) is added portionwise to a stirred mixture of 2-phenyl-5-methoxy-6,7-dichloro-1-indanone (4.61 g., 0.015 mole), iodoethane (15.5 ml., 0.15 mole), benzene (60 ml.) and dimethylformamide (60 ml.) under nitrogen in an ice-water bath. The reaction mixture is left to come to ambient temperature over one hour, then poured into water (1 l.), the benzene layer separated, dried over anhydrous magnesium sulfate and concentrated in vacuo to give 3.23 g. of 2-ethyl-2-phenyl-5-methoxy-6,7-dichloro-1-indanone which melts at 139°-141° C. on crystallization from benzene:hexane, 1:1.

후처리

  1. waitThe reaction mixture is left
  2. customthe benzene layer separated
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customto give 3.23 g
  6. customof 2-ethyl-2-phenyl-5-methoxy-6,7-dichloro-1-indanone which melts at 139°-141° C. on crystallization from benzene

출처 및 근거

ORD 기록
ord-6d7b9c41fbc143fe8b51fadf94aadfa9
출처 데이터셋
uspto-grants-1980_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04182764

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