Thionyl Chloride → HCID 59864270、化合物

HRID 1674497ノート

反応式

HRID 1674497 の反応式
[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]

参加物

5

反応物 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-butanol2 回

生成物 1

HCID 59864270HCID 59864270、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c8160d7e6c47422ab531dbab983a6874
出典データセット
uspto-grants-2011_08
特許番号
US08003638B2

反応ノート

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