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4-(4,4-Dimethoxybutyl)-5-oxo-[1,4]diazepane-1-carboxylic acid tert-butyl ester → 5-Oxo-4-(4-oxobutyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester

HRID 479350
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HRID 479350 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][C:12](=[O:15])[N:11]([CH2:16][CH2:17][CH2:18][CH:19](OC)[O:20]C)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]>C(O)(=O)C>[C:1]([O:5][C:6]([N:8]1[CH2:14][CH2:13][C:12](=[O:15])[N:11]([CH2:16][CH2:17][CH2:18][CH:19]=[O:20])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
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참가 물질

3

반응물 1

HCID 692244834-(4,4-Dimethoxybutyl)-5-oxo-[1,4]diazepane-1-carboxylic acid tert-butyl ester

생성물 1

HCID 113121495-Oxo-4-(4-oxobutyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester수율 32.9%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 4-(4,4-dimethoxybutyl)-5-oxo-[1,4]diazepane-1-carboxylic acid tert-butyl ester (3 g, 9.08 mmole) in glacial acetic acid containing 0.5 mL water (10 mL) was stirred at room temperature for 24 hours. The solution was concentrated at 35° C. under reduced pressure, and the residue was partitioned between saturated aqueous sodium bicarbonate and diethyl ether. The organic phase was dried (magnesium sulfate), concentrated, and the residue recrystallized from diethyl ether/hexane to give 5-oxo-4-(4-oxobutyl)-[1,4]diazepane-1-carboxylic acid tert-butyl ester (0.85 g,), m.p. 86-87° C.

후처리

  1. concentrationThe solution was concentrated at 35° C. under reduced pressure
  2. customthe residue was partitioned between saturated aqueous sodium bicarbonate and diethyl ether
  3. dry with materialThe organic phase was dried (magnesium sulfate)
  4. concentrationconcentrated
  5. customthe residue recrystallized from diethyl ether/hexane

출처 및 근거

ORD 기록
ord-1fef6879415b4e52a3333c529592df38
출처 데이터셋
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06645958B2

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