Hydrochloric Acid → HCID 67780906、化合物

HRID 1654458ノート

反応式

HRID 1654458 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-92ba4f8b4c814f228d13a9e8b08b4bb4
出典データセット
uspto-grants-1995_04
特許番号
US05407933

反応ノート

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