Thionyl Chloride → HCID 59864270, 화합물

HRID 1674497노트

반응식

HRID 1674497 반응식
[CH3:1][N:2]1[C:6]([C:7]2[CH:22]=[CH:21][C:10]3[CH2:11][CH2:12][N:13]([CH:16]([CH3:20])[CH2:17][CH2:18]O)[CH2:14][CH2:15][C:9]=3[CH:8]=2)=[CH:5][C:4]([CH3:23])=[N:3]1.S(Cl)([Cl:26])=O.C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl>[Cl:26][CH2:18][CH2:17][CH:16]([N:13]1[CH2:12][CH2:11][C:10]2[CH:21]=[CH:22][C:7]([C:6]3[N:2]([CH3:1])[N:3]=[C:4]([CH3:23])[CH:5]=3)=[CH:8][C:9]=2[CH2:15][CH2:14]1)[CH3:20]

참가 물질

5

반응물 3

HCID 24386Thionyl ChlorideHCID 516892Sodium BicarbonateHCID 598642713-[7-(1,3-Dimethyl-1H-pyrazol-5-yl)-1,2,4,5-tetrahydro-3H-3-benzazepin-3-yl]-1-butanol2회

생성물 1

HCID 59864270HCID 59864270, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a stirred solution of 3-[7-(1,3-dimethyl-1H-pyrazol-5-yl)-1,2,4,5-tetrahydro-3H-3-benzazepin-3-yl]-1-butanol (0.25 g) (intermediate 9) in chloroform (8 ml), at room temperature, thionyl chloride (0.11 ml) was added dropwise. After 2h, saturated aqueous sodium hydrogencarbonate (5 ml) was added, the reaction mixture was extracted with dichloromethane (15 ml), the organic phase dried with sodium sulphate and the solvent evaporated under reduced pressure. The crude product was purified by chromatography on silica gel with 80% cyclohexane-ethyl acetate to give the title compound (0.23 g) as a white solid.

후처리

  1. extractionthe reaction mixture was extracted with dichloromethane (15 ml)
  2. dry with materialthe organic phase dried with sodium sulphate
  3. customthe solvent evaporated under reduced pressure
  4. customThe crude product was purified by chromatography on silica gel with 80% cyclohexane-ethyl acetate

출처 및 근거

ORD 기록
ord-c8160d7e6c47422ab531dbab983a6874
출처 데이터셋
uspto-grants-2011_08
특허 번호
US08003638B2

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