Water → 3,5-Dichloro-3-(2-methoxyphenyl)indolin-2-one

HRID 552304

반응식

HRID 552304 반응식
S(Cl)([Cl:3])=O.[Cl:5][C:6]1[CH:7]=[C:8]2[C:12](=[CH:13][CH:14]=1)[NH:11][C:10](=[O:15])[C:9]2(O)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[O:22][CH3:23].N1C=CC=CC=1.O>C(Cl)Cl>[Cl:3][C:9]1([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[O:22][CH3:23])[C:8]2[C:12](=[CH:13][CH:14]=[C:6]([Cl:5])[CH:7]=2)[NH:11][C:10]1=[O:15]

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 24386Thionyl ChlorideHCID 219059555-Chloro-3-hydroxy-3-(2-methoxyphenyl)indolin-2-one

생성물 1

HCID 219059133,5-Dichloro-3-(2-methoxyphenyl)indolin-2-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

38 ml (0.518 mol) thionyl chloride were slowly added by drops to 100 g (0.345 mol) of the intermediate product 1a, 56 ml (0.695 mol) pyridine in 1 l methylene chloride at 0° C., and then stirred for approximately 30 minutes more. Then the reaction mixture was poured on to icy water and the organic phase was separated. This organic phase was then washed with water, dried and concentrated in a vacuum. The residue was treated with toluene a number of times and the organic solvent was removed in a vacuum each time. 79 g of the raw product were obtained and further reacted without further cleaning.

후처리

  1. customthe organic phase was separated
  2. washThis organic phase was then washed with water
  3. customdried
  4. concentrationconcentrated in a vacuum
  5. additionThe residue was treated with toluene a number of times
  6. customthe organic solvent was removed in a vacuum each time

출처 및 근거

ORD 기록
ord-6fd1ca05de294db6a5c76e158bcc37e6
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07951807B2

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