Water → Meridia

HRID 974530노트

반응식

HRID 974530 반응식
Cl.[CH3:2][N:3]([CH:5]([C:10]1([C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)[CH2:13][CH2:12][CH2:11]1)[CH2:6][CH:7]([CH3:9])[CH3:8])[CH3:4].[OH2:21]>>[OH2:21].[ClH:20].[CH3:2][N:3]([CH:5]([C:10]1([C:14]2[CH:15]=[CH:16][C:17]([Cl:20])=[CH:18][CH:19]=2)[CH2:13][CH2:12][CH2:11]1)[CH2:6][CH:7]([CH3:9])[CH3:8])[CH3:4]

참가 물질

3

반응물 2

HCID 962WaterHCID 64764Sibutramine Hydrochloride

생성물 1

HCID 64765Meridia

실험 절차

A sample (1 g) of N,N-dimethyl-1-[1-(4-chlorophenyl)cyclobutyl]-3-methylbutylamine hydrochloride which had been dehydrated in vacuo at 70° C. for 7 hours was treated with an organic solvent specified below (x ml) and then water (y ml) was added. The mixture was boiled and the resulting solution allowed to cool to ambient temperature and then stored at 4° C. for three hours. In Examples 10 and 11 the solution was stored at ambient temperature for 18 hours and crystallisation initiated by reducing the volume of the solution under a stream of air. A solid was collected by filtration, washed with the organic solvent and dried in vacuo at ambient temperature for 18 hours to give N,N-dimethyl-1-[1-(4-chlorophenyl)cyclobutyl]-3-methylbutylamine hydrochloride monohydrate the melting point of which is given below.

후처리

  1. additionwas treated with an organic solvent
  2. waitIn Examples 10 and 11 the solution was stored at ambient temperature for 18 hours
  3. customcrystallisation
  4. filtrationA solid was collected by filtration
  5. washwashed with the organic solvent
  6. customdried in vacuo at ambient temperature for 18 hours

출처 및 근거

ORD 기록
ord-9672808c8d854838b6237193a8891636
출처 데이터셋
uspto-grants-1991_11
특허 번호
US05068440

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