Hydrochloric Acid → HCID 67780906、化合物

HRID 2260149ノート

反応式

HRID 2260149 の反応式
[OH-].[Na+].[CH2:3]1[C@H:8]2[C:9]3[CH:21]=[CH:20][CH:19]=[CH:18][C:10]=3[CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[N:7]2[CH2:6][CH2:5][N:4]1[CH2:22][CH2:23][CH2:24][C:25]([O:27]CC)=[O:26].[ClH:30]>C(O)C>[ClH:30].[CH2:3]1[C@H:8]2[C:9]3[CH:21]=[CH:20][CH:19]=[CH:18][C:10]=3[CH2:11][C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=3[N:7]2[CH2:6][CH2:5][N:4]1[CH2:22][CH2:23][CH2:24][C:25]([OH:27])=[O:26]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 15287790HCID 15287790、化合物

生成物 1

HCID 67780906HCID 67780906、化合物収率 76%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

20 ml of a 10% w/v aqueous solution of sodium hydroxide were added to a solution of 14.34 g of ethyl (R)-4-(1,2,3,4,10,14b-hexahydrodibenzo[c,f]pyrazino[1.2-a]azepin-2-yl)butyrate (prepared as described in Example 5") in 100 ml of ethanol, and the resulting mixture was stirred at room temperature for 1 hour. At the end of this time, the pH of the reaction mixture was adjusted to a value of 2 by the addition of 10% w/v aqueous hydrochloric acid, and the solvent was removed by distillation under reduced pressure. The crystals which precipitated were collected by filtration and dried, to give the title compound, melting at 265°-268° C. (with decomposition), in a 76% yield.

後処理

  1. additionAt the end of this time, the pH of the reaction mixture was adjusted to a value of 2 by the addition of 10%
  2. customthe solvent was removed by distillation under reduced pressure
  3. customThe crystals which precipitated
  4. filtrationwere collected by filtration
  5. customdried

出典と根拠

ORDレコード
ord-845d02361f32441cb86e9af3510fe563
出典データセット
uspto-grants-1995_12
特許番号
US05476848

反応ノート

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