Water → 6,7-Dimethyl-5-methoxy-1,3-dihydro-2H-indole-2-one

HRID 1743397ノート

反応式

HRID 1743397 の反応式
[CH3:1][C:2]1[C:10]([CH3:11])=[C:9]2[C:5]([CH:6](SC)[C:7](=[O:12])[NH:8]2)=[CH:4][C:3]=1[O:15][CH3:16].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O.C1(C)C(S(O)(=O)=O)=CC=CC=1.O>ClCCl>[CH3:1][C:2]1[C:10]([CH3:11])=[C:9]2[C:5]([CH2:6][C:7](=[O:12])[NH:8]2)=[CH:4][C:3]=1[O:15][CH3:16]

参加物

6

反応物 4

HCID 962WaterHCID 11776TriphenylphosphineHCID 124969952-Methylbenzenesulfonic acid hydrateHCID 222380776,7-Dimethyl-5-methoxy-3-(methylthio)-1,3-dihydro-2H-indole-2-one

生成物 1

HCID 222380866,7-Dimethyl-5-methoxy-1,3-dihydro-2H-indole-2-one収率 72.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 6,7-dimethyl-5-methoxy-3(methylthio)-1,3-dihydro-2H-indole-2-one (30 g, 126 mmol) in dichloromethane (600 mL) were added triphenylphosphine (40 g, 153 mmol) and toluenesulfonic acid monohydrate (29 g, 153 mmol) at room temperature, and the mixture was stirred for 3 hours. The reaction solution was poured into cool water, and the precipitated crystals were filtered. The crystals were washed with dichloromethane and water to obtain 17.5 g of the title compound.

後処理

  1. additionThe reaction solution was poured
  2. filtrationthe precipitated crystals were filtered
  3. washThe crystals were washed with dichloromethane and water

出典と根拠

ORDレコード
ord-ad8c36e386b34d36a1b6ea7ae5f1c0fb
出典データセット
uspto-grants-2006_03
特許番号
US07008940B1

反応ノート

読み込み中…