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Phosgene → 7-[6-(1H-imidazol-2-yl)pyridin-3-yl]-2,3-dihydro-1,4-benzoxazepin-4(5H)-carbonyl chloride

HRID 473913
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인쇄 미리보기

반응식

HRID 473913 반응식
[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]1[N:11]=[CH:10][C:9]([C:12]2[CH:13]=[CH:14][C:15]3[O:21][CH2:20][CH2:19][NH:18][CH2:17][C:16]=3[CH:22]=2)=[CH:8][CH:7]=1.C(N(C(C)C)CC)(C)C.[C:32](Cl)([Cl:34])=[O:33]>ClCCl.C1(C)C=CC=CC=1>[NH:1]1[CH:5]=[CH:4][N:3]=[C:2]1[C:6]1[N:11]=[CH:10][C:9]([C:12]2[CH:13]=[CH:14][C:15]3[O:21][CH2:20][CH2:19][N:18]([C:32]([Cl:34])=[O:33])[CH2:17][C:16]=3[CH:22]=2)=[CH:8][CH:7]=1
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참가 물질

6

반응물 3

HCID 6371PhosgeneHCID 81531DiisopropylethylamineHCID 675137447-[6-(1H-imidazol-2-yl)pyridin-3-yl]-2,3,4,5-tetrahydro-1,4-benzoxazepine

생성물 1

HCID 866720357-[6-(1H-imidazol-2-yl)pyridin-3-yl]-2,3-dihydro-1,4-benzoxazepin-4(5H)-carbonyl chloride

시약·촉매·용매 2

HCID 1140Toluene용매
HCID 6344
Dichloromethane
용매

실험 절차

The 7-[6-(1H-imidazol-2-yl)pyridin-3-yl]-2,3,4,5-tetrahydro-1,4-benzoxazepine as obtained in step 3 was dissolved in dichloromethane (2 mL), diisopropylethylamine (0.12 mL, 0.65 mmol) was added, followed by addition of phosgene (0.07 mL of a 20% solution in toluene, 0.13 mmol). The reaction mixture was stirred at room temperature for 30 min and then concentrated to afford crude 7-[6-(1H-imidazol-2-yl)pyridin-3-yl]-2,3-dihydro-1,4-benzoxazepin-4(5H)-carbonyl chloride.

후처리

  1. concentrationconcentrated

출처 및 근거

ORD 기록
ord-7e4ea96e92de410da31d1c2176baa87c
출처 데이터셋
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08637499B2

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