Hydrochloric Acid → N-(3-Pyridinylmethyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxamide

HRID 1830093노트

반응식

HRID 1830093 반응식
COC([N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[CH2:9][N:8]2[C:16]([C:19]([NH:21][CH2:22][C:23]3[CH:24]=[N:25][CH:26]=[CH:27][CH:28]=3)=[O:20])=[CH:17][CH:18]=[C:7]2[CH2:6]1)=O.C(=O)([O-])[O-].[K+].[K+].O.Cl>CO>[N:25]1[CH:26]=[CH:27][CH:28]=[C:23]([CH2:22][NH:21][C:19]([C:16]2[N:8]3[C:7]([CH2:6][NH:5][C:11]4[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=4[CH2:9]3)=[CH:18][CH:17]=2)=[O:20])[CH:24]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 11430Potassium CarbonateHCID 2205365210-(Methoxycarbonyl)-N-(pyridin-3-ylmethyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxamide

생성물 1

HCID 22053658N-(3-Pyridinylmethyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxamide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 10-(methoxycarbonyl)-N-(pyridin-3-ylmethyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxamide (5 mmol) of Step B in methanol (50 mL) was treated with potassium carbonate and stirred at room temperature overnight. Water was then added to the solution and the pH adjusted to 6 with 6N hydrochloric acid. The solution was extracted with ethyl acetate, and the combined organic layers were dried over anhydrous magnesium sulfate, and evaporated to dryness. The residual oil was triturated with ethyl acetate and hexane to yield the title compound as a powder.

후처리

  1. extractionThe solution was extracted with ethyl acetate
  2. dry with materialthe combined organic layers were dried over anhydrous magnesium sulfate
  3. customevaporated to dryness
  4. customThe residual oil was triturated with ethyl acetate and hexane

출처 및 근거

ORD 기록
ord-aa39361e44fa45ee9f340f083efb44c7
출처 데이터셋
uspto-grants-2006_06
특허 번호
US07064120B2

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