Methanol → HCID 22053989, 화합물

HRID 1830126

반응식

HRID 1830126 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 22053989HCID 22053989, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d2b151c39d9a41da90bb419d88fb61a9
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07064123B1

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