Triethylamine → HCID 22632361, 화합물

HRID 2417493노트

반응식

HRID 2417493 반응식
[Cl:1][C:2]1[CH:38]=[CH:37][C:5]([C:6]([N:8]2[CH2:14][C:13]3[CH:15]=[CH:16][C:17]([C:19](O)=[O:20])=[CH:18][C:12]=3[N:11]([CH2:22][C:23]3[CH:28]=[CH:27][C:26]([C:29]([N:31]4[CH2:35][CH2:34][CH2:33][CH2:32]4)=[O:30])=[CH:25][CH:24]=3)[C:10](=[O:36])[CH2:9]2)=[O:7])=[CH:4][CH:3]=1.C(N(CC)CC)C.ClC(OCC)=O.[BH4-].[Na+]>C1COCC1.C(OCC)(=O)C>[OH:20][CH2:19][C:17]1[CH:16]=[CH:15][C:13]2[CH2:14][N:8]([C:6](=[O:7])[C:5]3[CH:4]=[CH:3][C:2]([Cl:1])=[CH:38][CH:37]=3)[CH2:9][C:10](=[O:36])[N:11]([CH2:22][C:23]3[CH:28]=[CH:27][C:26]([C:29]([N:31]4[CH2:35][CH:34]=[CH:33][CH2:32]4)=[O:30])=[CH:25][CH:24]=3)[C:12]=2[CH:18]=1

참가 물질

7

반응물 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 4311764Sodium borohydrideHCID 22632665HCID 22632665, 화합물

생성물 1

HCID 22632361HCID 22632361, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

650 mg (1.22 mmol) of 4-(4-chlorobenzoyl)-2-oxo-1-[4-(1-pyrrolidinecarbonyl)benzyl]-2,3,4,5-tetrahydro-1H-benzo[e][1,4]-diazepine-8-carboxylic acid was dissolved in 50 ml of THF. 0.42 ml (2.4 mmol) of triethylamine and 0.15 ml (0.63 mmol) of ethyl chloroformate were added to the obtained solution under cooling with ice, and they were stirred for 30 minutes. A piece of ice was added to the obtained mixture, and then 92 mg (1.1 mmol) of sodium borohydride was added thereto. The temperature was elevated to room temperature, and the obtained mixture was stirred overnight. After the treatment with ethyl acetate as the extracting solvent, the title compound was obtained.

후처리

  1. temperatureunder cooling with ice, and they
  2. additionA piece of ice was added to the obtained mixture
  3. customwas elevated to room temperature
  4. stirringthe obtained mixture was stirred overnight

출처 및 근거

ORD 기록
ord-c8a249b27299459aa9c640db50fb345d
출처 데이터셋
uspto-grants-2004_11
특허 번호
US06825191B2

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