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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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tert-butyl 1-(3-methylbut-2-enoyl)-2,3-dihydro-1H-benzo[e][1,4]diazepine-4(5H)-carboxylate → tert-butyl 8,8-dimethyl-6-oxo-3,4,7,8-tetrahydro-1H-[1,4]diazepino[6,7,1-ij]quinoline-2(6H)-carboxylate

HRID 1754541
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HRID 1754541 반응식
[CH3:1][C:2]([CH3:24])=[CH:3][C:4]([N:6]1[C:12]2[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=2[CH2:10][N:9]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:8][CH2:7]1)=[O:5]>[Hg]>[CH3:1][C:2]1([CH3:24])[C:13]2[C:12]3=[C:11]([CH2:10][N:9]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:8][CH2:7][N:6]3[C:4](=[O:5])[CH2:3]1)[CH:16]=[CH:15][CH:14]=2
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참가 물질

3

반응물 1

HCID 86712747tert-butyl 1-(3-methylbut-2-enoyl)-2,3-dihydro-1H-benzo[e][1,4]diazepine-4(5H)-carboxylate

생성물 1

HCID 86712748tert-butyl 8,8-dimethyl-6-oxo-3,4,7,8-tetrahydro-1H-[1,4]diazepino[6,7,1-ij]quinoline-2(6H)-carboxylate수율 61.1%

시약·촉매·용매 1

HCID 23931Mercury촉매

실험 절차

A solution of 0.33 g (1.0 mmol) of tert-butyl 1-(3-methylbut-2-enoyl)-2,3-dihydro-1H-benzo[e][1,4]diazepine-4(5H)-carboxylate of step 1.1 was irradiated with a 150 W mercury lamp in a immersion well reactor with a pyrex filter in 20 mL of acetone until completion of the reaction monitored by liquid chromatography. The solution was concentrated in vacuo and the residue was purified by column chromatography on silica (eluent: 10-30% ethyl acetate in heptane) to yield 202 mg of the title compound as a beige solid.

후처리

  1. filtrationfilter in 20 mL of acetone until completion of the reaction
  2. concentrationThe solution was concentrated in vacuo
  3. customthe residue was purified by column chromatography on silica (eluent: 10-30% ethyl acetate in heptane)

출처 및 근거

ORD 기록
ord-9110e5e19b7f437b86b2780d6c91a2ce
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09169253B2

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