Hydrochloric Acid → HCID 67780906, 화합물

HRID 2260149노트

반응식

HRID 2260149 반응식
[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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 15287790HCID 15287790, 화합물

생성물 1

HCID 67780906HCID 67780906, 화합물수율 76%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-845d02361f32441cb86e9af3510fe563
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05476848

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