Methanol → HCID 22053989、化合物

HRID 1830126ノート

反応式

HRID 1830126 の反応式
[CH2:1]=[C:2]([CH2:6][C:7]([N:9]1[CH2:14][CH2:13][O:12][CH2:11][CH2:10]1)=[O:8])[C:3]([OH:5])=[O:4].[F:15][C:16]([F:26])([F:25])[C:17]1[CH:24]=[CH:23][CH:22]=[CH:21][C:18]=1[CH2:19]S.CO.O[O:30][S:31]([O-:33])=O.[K+]>CN(C=O)C.CN(C1C=CN=CC=1)C>[N:9]1([C:7](=[O:8])[CH2:6][CH:2]([CH2:1][S:31]([CH2:19][C:18]2[CH:21]=[CH:22][CH:23]=[CH:24][C:17]=2[C:16]([F:15])([F:25])[F:26])(=[O:33])=[O:30])[C:3]([OH:5])=[O:4])[CH2:10][CH2:11][O:12][CH2:13][CH2:14]1

参加物

7

反応物 4

HCID 887MethanolHCID 27614232-(Trifluoromethyl)phenylmethanethiolHCID 220540222-Methylene4-morpholin-4-yl-4-oxo-butyric acidHCID 23707502Potassium hydroxy sulfite

生成物 1

HCID 22053989HCID 22053989、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 2-methylene-4-morpholin-4-yl-4-oxo-butyric acid (2 g, 10.03 mmol), in DMF (5 mL), 2-trifluoromethylbenzyl mercaptan (1.93 g, 10.03 mmol) and DMAP (122 mg, 1.0 mmol) was stirred at ambient temperature for 16 hours. Methanol (200 mL) and a saturated aqueous solution of Oxone® (20 g, 32.5 mmol) were added with continued stirring for 2 hours. Methanol was removed under vacuum and the aqueous residue was diluted with 200 mL of water. The crystallized product was filtered, washed with water, and dried under vacuum to yield 4-morpholin-4-yl-4-oxo-2-(2-trifluoromethyl-benzylsulfonylmethyl)-butyric acid (0.95 g) as a white solid.

後処理

  1. customMethanol was removed under vacuum
  2. additionthe aqueous residue was diluted with 200 mL of water
  3. filtrationThe crystallized product was filtered
  4. washwashed with water
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-d2b151c39d9a41da90bb419d88fb61a9
出典データセット
uspto-grants-2006_06
特許番号
US07064123B1

反応ノート

読み込み中…