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

HRID 552304

反応式

HRID 552304 の反応式
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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6fd1ca05de294db6a5c76e158bcc37e6
出典データセット
uspto-grants-2011_05
特許番号
US07951807B2

関連ノート

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