Water → (R)-N-[1-[(3-chlorothien-2-yl)methyl]propyl]-4-methylbenzenesulfonamide

HRID 2302086ノート

反応式

HRID 2302086 の反応式
[Li].[Cl:2][C:3]1[CH:7]=[CH:6][S:5][C:4]=1[CH2:8][C@H:9]([NH:12][S:13]([C:16]1[CH:21]=[CH:20][C:19]([CH3:22])=[CH:18][CH:17]=1)(=[O:15])=[O:14])[CH2:10][CH3:11].O>CO>[Cl:2][C:3]1[CH:7]=[CH:6][S:5][C:4]=1[CH2:8][C@H:9]([NH:12][S:13]([C:16]1[CH:17]=[CH:18][C:19]([CH3:22])=[CH:20][CH:21]=1)(=[O:15])=[O:14])[CH2:10][CH3:11]

参加物

4

反応物 2

HCID 962WaterHCID 69848256(R)-N-[1-[(3-chlorothien-2-yl)methyl]propyl]-4-methylbenzenesulfonamide lithium salt

生成物 1

HCID 11002430(R)-N-[1-[(3-chlorothien-2-yl)methyl]propyl]-4-methylbenzenesulfonamide収率 95%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
65 °C

実験手順

A mixture of 50.0 g (0.143 mol) of (R)-N-[1-[(3-chlorothien-2-yl )methyl]propyl]-4-methylbenzenesulfonamide lithium salt, prepared as described in PCT/US97/15729, in 50 g methanol is heated with stirring at 65° C. until dissolution of the solids is completed. The solution is cooled to 60° C. and 85 g water is added to the mixture dropwise. The mixture is stirred for 1.5 hours and then cooled to 20° C. The solids are isolated by filtration. Drying under vacuum with nitrogen bleed affords 46.6 g (95%) of the free base (R)-N-[1-[(3-chlorothien-2-yl)methyl]propyl]-4-methylbenzenesulfonamide.

後処理

  1. customprepared
  2. temperatureis heated
  3. temperatureThe solution is cooled to 60° C.
  4. stirringThe mixture is stirred for 1.5 hours
  5. temperaturecooled to 20° C
  6. customThe solids are isolated by filtration
  7. customDrying under vacuum with nitrogen

出典と根拠

ORDレコード
ord-558184f185874d8ca70ae827d7e11278
出典データセット
uspto-grants-2002_08
特許番号
US06429315B1

反応ノート

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