Water → Meridia

HRID 974530ノート

反応式

HRID 974530 の反応式
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]

参加物

3

反応物 2

HCID 962WaterHCID 64764Sibutramine Hydrochloride

生成物 1

HCID 64765Meridia

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9672808c8d854838b6237193a8891636
出典データセット
uspto-grants-1991_11
特許番号
US05068440

反応ノート

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