Traboxopine → HCID 14555943、化合物

HRID 1164786ノート

反応式

HRID 1164786 の反応式
[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[O:6][CH2:7][O:8][C:9]3[CH:22]=[CH:21][CH:20]=[CH:19][C:10]=3[N:11]([CH2:12][CH:13]([CH3:18])[CH2:14][N:15]([CH3:17])[CH3:16])[C:4]=2[CH:3]=1.[C:25]([OH:34])(=[O:33])[C@@H:26]([C@H:28]([C:30]([OH:32])=[O:31])[OH:29])[OH:27]>O>[C:30]([C@@H:28]([C@H:26]([C:25]([OH:34])=[O:33])[OH:27])[OH:29])([OH:32])=[O:31].[Cl:1][C:2]1[CH:24]=[CH:23][C:5]2[O:6][CH2:7][O:8][C:9]3[CH:22]=[CH:21][CH:20]=[CH:19][C:10]=3[N:11]([CH2:12][CH:13]([CH3:18])[CH2:14][N:15]([CH3:17])[CH3:16])[C:4]=2[CH:3]=1

参加物

4

反応物 2

HCID 129812TraboxopineHCID 444305L-Tartaric acid

生成物 1

HCID 14555943HCID 14555943、化合物収率 70%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

From the dichloromethane filtrate obtained in Example 3, section (A), the base is deliberated by the method of Example 1, section (B). To the residual syrup weighing 21.5 g, 9.3 g 0.063 moles of L(+)-tartaric acid are added in 85 CM3 of water. At first, a solution is obtained that is stirred for several hours. The (-)-base L(+)-tartrate precipitated is filtered, suspended in cold water, then filtered, suspended and filtered again. Thus, 17.5 g (70.0%) of (-)-2-chloro-12-(3-dimethylamino-2-methylpropyl)-12H-dibenzo[d,g][1,3,6]dioxazocine L(+)-tartrate are obtained, m.p.: 109°-114° C.

後処理

  1. customAt first, a solution is obtained
  2. customThe (-)-base L(+)-tartrate precipitated
  3. filtrationis filtered
  4. filtrationfiltered
  5. filtrationfiltered again

出典と根拠

ORDレコード
ord-fce6a8337c934c9db4592a39aa34f74f
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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