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Triethylamine → HCID 178421979, 화합물

HRID 1040560
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HRID 1040560 반응식
Cl.[NH:2]([C:4]([C:6]1([NH:9][C:10]([C:12]2([NH:15][C:16]([C:18]3[N:22]4[C@@:23]([CH2:36][C:37]5[CH:42]=[CH:41][C:40]([C:43]#[N:44])=[CH:39][CH:38]=5)([CH3:35])[C:24](=[O:34])[N:25]([C:26]5[CH:31]=[C:30]([Cl:32])[CH:29]=[C:28]([Cl:33])[CH:27]=5)[C:21]4=[N:20][CH:19]=3)=[O:17])[CH2:14][CH2:13]2)=[O:11])[CH2:8][CH2:7]1)=O)[NH2:3].Cl.C(O[C:49]([CH:51]1[CH2:53][CH2:52]1)=[NH:50])C.CCN(CC)CC>CN(C=O)C>[CH:51]1([C:49]2[NH:50][C:4]([C:6]3([NH:9][C:10]([C:12]4([NH:15][C:16]([C:18]5[N:22]6[C@@:23]([CH2:36][C:37]7[CH:38]=[CH:39][C:40]([C:43]#[N:44])=[CH:41][CH:42]=7)([CH3:35])[C:24](=[O:34])[N:25]([C:26]7[CH:31]=[C:30]([Cl:32])[CH:29]=[C:28]([Cl:33])[CH:27]=7)[C:21]6=[N:20][CH:19]=5)=[O:17])[CH2:13][CH2:14]4)=[O:11])[CH2:7][CH2:8]3)=[N:2][N:3]=2)[CH2:53][CH2:52]1
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참가 물질

5

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HCID 8471TriethylamineHCID 20026660Ethyl cyclopropanecarboximidate hydrochlorideHCID 67389773(R)-5-(4-cyano-benzyl)-7-(3,5-dichloro-phenyl)-5-methyl-6-oxo-6,7-dihydro-5H-imidazo-[1,2-a]imidazole-3-carboxylic acid [1-(1-hydrazinocarbonyl-cyclopropylcarbamoyl)-cyclopropyl]-amide hydrochloride

생성물 1

HCID 178421979HCID 178421979, 화합물수율 28%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

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온도
140 °C

실험 절차

To a solution of (R)-5-(4-cyano-benzyl)-7-(3,5-dichloro-phenyl)-5-methyl-6-oxo-6,7-dihydro-5H-imidazo[1,2-a]imidazole-3-carboxylic acid [1-(1-hydrazinocarbonyl-cyclopropylcarbamoyl)-cyclopropyl]-amide hydrochloride (0.080 g, 0.12 mmol) and cyclopropanecarboximidic acid ethyl ester hydrochloride (0.018 g, 0.12 mmol) in DMF (1 mL) was added Et3N (0.051 mL, 0.37 mmol). The reaction was heated in a microwave at 140° C. for 45 min and then at 180° C. for 1.5 h. The mixture was cooled to room temperature and purified via reverse-phase HPLC to give (R)-5-(4-cyano-benzyl)-7-(3,5-dichloro-phenyl)-5-methyl-6-oxo-6,7-dihydro-5H-imidazo[1,2-a]imidazole-3-carboxylic acid {1-[1-(5-cyclopropyl-4H-1,2,4-triazol-3-yl)-cyclopropylcarbamoyl]-cyclopropyl}-amide (0.022 g, 28%) as a white solid, m/z 670.8 [M+1]+.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. custompurified via reverse-phase HPLC

출처 및 근거

ORD 기록
ord-63f95d0d4df448858bc1d5f5d3444f8d
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08552205B2

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