Water → Traboxopine

HRID 1164783ノート

反応式

HRID 1164783 の反応式
C([C@@H]([C@H](C(O)=O)O)O)(O)=O.[Cl:11][C:12]1[CH:34]=[CH:33][C:15]2[O:16][CH2:17][O:18][C:19]3[CH:32]=[CH:31][CH:30]=[CH:29][C:20]=3[N:21]([CH2:22][CH:23]([CH3:28])[CH2:24][N:25]([CH3:27])[CH3:26])[C:14]=2[CH:13]=1.O>ClCCl>[Cl:11][C:12]1[CH:34]=[CH:33][C:15]2[O:16][CH2:17][O:18][C:19]3[CH:32]=[CH:31][CH:30]=[CH:29][C:20]=3[N:21]([CH2:22][CH:23]([CH3:28])[CH2:24][N:25]([CH3:27])[CH3:26])[C:14]=2[CH:13]=1

参加物

4

反応物 2

HCID 962WaterHCID 14555943HCID 14555943、化合物

生成物 1

HCID 129812Traboxopine収率 84.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a stirred mixture of 19.0 g (0.038 moles) of (-)-2-chloro-12-(3-dimethylamino-2-methylpropyl)-12H-dibenzo[d,g][1,3,6]dioxazocine L(+)-tartrate, 100 cm3 of water and 100 cm3 of dichloromethane 25 percent aqueous ammonia is added until a pH value of 10. The mixture is stirred for further 30 minutes, the organic phase is separated and the solvent is removed under reduced pressure. The viscous residue is dissolved in 28 cm3 of isopropanol, cooled to 0° C. and the crystals are filtered. 11.1 g 84.0% of the title compound are obtained, m.p.: 92°-95° C.

後処理

  1. additionis added until a pH value of 10
  2. customthe organic phase is separated
  3. customthe solvent is removed under reduced pressure
  4. dissolutionThe viscous residue is dissolved in 28 cm3 of isopropanol
  5. filtrationthe crystals are filtered

出典と根拠

ORDレコード
ord-62a4da17b0f84c29917788d7ef6e96d0
出典データセット
uspto-grants-1990_03
特許番号
US04906622

反応ノート

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