Cyclopropylmethylsulphinic acid → HCID 22054098、化合物

HRID 1796134

反応式

HRID 1796134 の反応式
[CH:1]1([CH2:4][S:5]([OH:7])=[O:6])[CH2:3][CH2:2]1.[CH2:8]=[C:9]([CH2:13][C:14]([N:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1)=[O:15])[C:10]([OH:12])=[O:11]>C1(C)C=CC=CC=1.C(#N)C>[CH:1]1([CH2:4][S:5]([CH2:8][CH:9]([CH2:13][C:14]([N:16]2[CH2:17][CH2:18][O:19][CH2:20][CH2:21]2)=[O:15])[C:10]([OH:12])=[O:11])(=[O:7])=[O:6])[CH2:3][CH2:2]1

参加物

5

反応物 2

HCID 17937320Cyclopropylmethylsulphinic acidHCID 220540222-Methylene4-morpholin-4-yl-4-oxo-butyric acid

生成物 1

HCID 22054098HCID 22054098、化合物収率 40.1%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
85 °C

実験手順

To a solution of cyclopropylmethylsulphinic acid (1.8 g, 15 mmol) in anhydrous toluene (45 mL) and anhydrous acetonitrile (9 mL) was added 2-Methylene4-morpholin-4-yl-4-oxo-butyric acid (2.98 g, 15 mmol). The resulting solution was warmed to 85° C. and stirred at this temperature for 4.5 h. The heterogeneous reaction mixture is then allowed to cool to room temperature then concentrated under reduced pressure. The residue is then purified by flash chromatography eluting with 7% methanol in dichloromethane to give 2-Cyclopropylmethanesulfonylmethyl-4-morpholin-4-yl-4-oxo-butyric acid (1.92 g) as viscous oil which was re crystallized from hot ethyl acetate to give a white solid.

後処理

  1. temperatureto cool to room temperature
  2. concentrationthen concentrated under reduced pressure
  3. customThe residue is then purified by flash chromatography
  4. washeluting with 7% methanol in dichloromethane

出典と根拠

ORDレコード
ord-eeb3f2e7ab404a5f96dc1a8bc5ff6cc1
出典データセット
uspto-grants-2006_04
特許番号
US07030116B2

関連ノート

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