Dimethylformamide → HCID 178451667, 화합물

HRID 13346

반응식

HRID 13346 반응식
[NH:1]1[CH:5]=[CH:4][C:3]([CH:6]=O)=[N:2]1.CN(C)C=O.[NH2:13][C:14]1[C:19]([NH2:20])=[CH:18][C:17]([CH:21]2[CH2:25][CH2:24][CH2:23][N:22]2[C:26]([O:28][C:29]([CH3:32])([CH3:31])[CH3:30])=[O:27])=[C:16]([O:33][C:34]2[CH:39]=[CH:38][C:37]([S:40]([CH3:43])(=[O:42])=[O:41])=[CH:36][CH:35]=2)[CH:15]=1>C(OCC)(=O)C>[CH3:43][S:40]([C:37]1[CH:38]=[CH:39][C:34]([O:33][C:16]2[C:17]([CH:21]3[CH2:25][CH2:24][CH2:23][N:22]3[C:26]([O:28][C:29]([CH3:30])([CH3:32])[CH3:31])=[O:27])=[CH:18][C:19]3[NH:20][C:6]([C:3]4[CH:4]=[CH:5][NH:1][N:2]=4)=[N:13][C:14]=3[CH:15]=2)=[CH:35][CH:36]=1)(=[O:42])=[O:41]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 122183831H-Pyrazole-3-carbaldehydeHCID 23145168t-Butyl 2-(4,5-diamino-2-(4-methanesulfonyl-phenoxy)phenyl)-pyrrolidine-1-carboxylate

생성물 1

HCID 178451667HCID 178451667, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
90 °C

실험 절차

10.0 mg of 1H-pyrazole-3-carboxaldehyde was added to an N,N-dimethylformamide (1 ml) solution of 49.0 mg of t-butyl 2-(4,5-diamino-2-(4-methanesulfonyl-phenoxy)-phenyl)-pyrrolidine-1-carboxylate obtained in Example 306 (step 3), and the reaction liquid was stirred overnight at 90° C. After cooled, the reaction liquid was diluted with ethyl acetate, washed with saturated saline, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting residue was purified through partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=9/1) to obtain the entitled compound as a brown solid.

후처리

  1. customthe reaction liquid
  2. temperatureAfter cooled
  3. customthe reaction liquid
  4. washwashed with saturated saline
  5. dry with materialdried with anhydrous magnesium sulfate
  6. customThe solvent was evaporated away under reduced pressure
  7. customthe resulting residue was purified
  8. customthrough partitioning thin-layer chromatography (Kieselgel™ 60F254, Art 5744 (by Merck), chloroform/methanol=9/1)

출처 및 근거

ORD 기록
ord-e88808f8ef4a4eb29b06851b1f3a5734
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

연결된 노트

불러오는 중…