Diisopropylethylamine → HCID 178502434, 화합물

HRID 1625528노트

반응식

HRID 1625528 반응식
[I:1][C:2]1[CH:16]=[CH:15][C:5]2[NH:6][C:7]([C@@H:9]3[CH2:13][C@H:12]([CH3:14])[CH2:11][NH:10]3)=[N:8][C:4]=2[CH:3]=1.[CH3:17][O:18][C:19]([NH:21][C@@H:22]([CH:26]([CH3:28])[CH3:27])[C:23](O)=[O:24])=[O:20].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C.O>[I:1][C:2]1[CH:16]=[CH:15][C:5]2[NH:6][C:7]([C@@H:9]3[CH2:13][C@H:12]([CH3:14])[CH2:11][N:10]3[C:23]([C@@H:22]([NH:21][C:19](=[O:20])[O:18][CH3:17])[CH:26]([CH3:28])[CH3:27])=[O:24])=[N:8][C:4]=2[CH:3]=1

참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 10942966(2S)-2-((methoxycarbonyl)amino)-3-methylbutanoic acidHCID 178461565HCID 178461565, 화합물

생성물 1

HCID 178502434HCID 178502434, 화합물수율 81%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To 5-iodo-2-[(2S,4S)-4-methylpyrrolidin-2-yl]-1H-benzimidazole (2.29 g, 7.00 mmol) and (2S)-2-(methoxycarbonylamino)-3-methyl-butanoic acid (1.49 g, 7.70 mmol) in DMF is added HATU (3.46 g, 9.1 mmol) and DIPEA (2.4 mL, 14.0 mmol) at rt. The reaction mixture is stirred at rt overnight. To the reaction mixture is added water (350 mL) with fast stirring upon which a white solid precipitated out. The solid is suction filtered and dried under vacuum to give methyl N-[(1S)-1-[(2S,4S)-2-(5-iodo-1H-benzimidazol-2-yl)-4-methyl-pyrrolidine-1-carbonyl]-2-methyl-propyl]carbamate (2.73 g, 81%).

후처리

  1. stirringwith fast stirring upon which a white solid
  2. customprecipitated out
  3. filtrationfiltered
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-ba7fa9351693486f84bb80b6fc2c159b
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08779156B2

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