Water → Traboxopine

HRID 1164783노트

반응식

HRID 1164783 반응식
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

참가 물질

4

반응물 2

HCID 962WaterHCID 14555943HCID 14555943, 화합물

생성물 1

HCID 129812Traboxopine수율 84.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-62a4da17b0f84c29917788d7ef6e96d0
출처 데이터셋
uspto-grants-1990_03
특허 번호
US04906622

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