Water → HCID 44717450, 화합물

HRID 1748290

반응식

HRID 1748290 반응식
[F:1][C:2]([F:7])([CH2:5][OH:6])[CH2:3][OH:4].C(N([CH2:13][CH3:14])CC)C.[CH3:15][C:16]1[CH:21]=[CH:20][C:19]([S:22](Cl)(=[O:24])=[O:23])=[CH:18][CH:17]=1.[OH2:26]>C(Cl)Cl>[CH3:15][C:16]1[CH:21]=[CH:20][C:19]([S:22]([O:4][CH2:3][C:2]([F:7])([F:1])[CH2:5][O:6][S:22]([C:19]2[CH:20]=[CH:21][C:13]([CH3:14])=[CH:17][CH:18]=2)(=[O:23])=[O:26])(=[O:24])=[O:23])=[CH:18][CH:17]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 957442,2-Difluoropropane-1,3-diol

생성물 1

HCID 44717450HCID 44717450, 화합물수율 71%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 2,2-difluoropropane-1,3-diol (2.5 g, 22.3 mmol) in CH2Cl2 (100 mL) is added triethylamine (14.3 mL, 111.5 mmol) followed by 4-methyl-benzenesulfonyl chloride (12.8 g, 66.9 mmol). The reaction mixture is stirred for 16 h at room temperature. Water (35 mL) is added and the organic layer is separated and washed with more water (2×35 mL). The organic layer is concentrated and the crude compound is purified by flash column chromatography using EtOAc in heptane to afford the title compound (6.7 g, 71%).

후처리

  1. customthe organic layer is separated
  2. washwashed with more water (2×35 mL)
  3. concentrationThe organic layer is concentrated
  4. customthe crude compound is purified by flash column chromatography

출처 및 근거

ORD 기록
ord-535cedb8697a4187928440bbe451479b
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09150577B2

연결된 노트

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