Ammonia → (S)-(+)-N,N-Dimethyl-3-(1-naphthalenyloxy)-3-(2-thienyl)propanamine

HRID 2388362

反応式

HRID 2388362 の反応式
C([C@@](C(O)=O)(O)[C@@](C(=O)C1C=CC(OC)=CC=1)(O)C(O)=O)(=O)C1C=CC(OC)=CC=1.[CH3:31][N:32]([CH3:52])[CH2:33][CH2:34][C@H:35]([O:41][C:42]1[C:51]2[C:46](=[CH:47][CH:48]=[CH:49][CH:50]=2)[CH:45]=[CH:44][CH:43]=1)[C:36]1[S:37][CH:38]=[CH:39][CH:40]=1.O.N>ClCCl>[CH3:52][N:32]([CH3:31])[CH2:33][CH2:34][C@H:35]([O:41][C:42]1[C:51]2[C:46](=[CH:47][CH:48]=[CH:49][CH:50]=2)[CH:45]=[CH:44][CH:43]=1)[C:36]1[S:37][CH:38]=[CH:39][CH:40]=1

参加物

5

反応物 3

HCID 222AmmoniaHCID 962WaterHCID 131729950(s)-n,n-Dimethyl-3-(1-naphthalenyloxy)-3-(2-thienyl)propanamine di-p-anisoyl-l-tartarate salt

生成物 1

HCID 9818212(S)-(+)-N,N-Dimethyl-3-(1-naphthalenyloxy)-3-(2-thienyl)propanamine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The (S)—N,N-dimethyl-3-(1-naphthalenyloxy)-3-(2-thienyl)propanamine di-p-anisoyl-L-tartarate salt (9a) (100 gm) was added to biphasic solvent mixture of water (500 ml) and dichloromethane (250 ml). To the slurry aqueous ammonia was added to adjust the pH to 10.8 and stirred further for 15-30 minutes. Organic layer was separated, washed with water, brine and concentrated to get thick oily mass of (S)-(+)-N,N-dimethyl-3-(1-naphthalenyloxy)-3-(2-thienyl)propanamine (6a). Yield: 44 gm.

後処理

  1. customOrganic layer was separated
  2. washwashed with water, brine
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-be9844340aca479bb9f7311c5480e66c
出典データセット
uspto-grants-2012_09
特許番号
US08269023B2

関連ノート

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