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N-methyl-2-pyrrolidone → HCID 178521288, 화합물

HRID 900730
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HRID 900730 반응식
CS[C:3]1[NH:7][N:6]=[C:5]([C:8]2[CH:13]=[CH:12]N=C[CH:9]=2)[N:4]=1.[NH2:14][CH2:15][C:16]([NH:18][C:19]1[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[CH:20]=1)=[O:17].[CH3:26][N:27]1C(=O)CCC1>>[Cl:25][C:21]1[CH:20]=[C:19]([NH:18][C:16](=[O:17])[CH2:15][NH:14][C:3]2[NH:7][N:6]=[C:5]([C:8]3[CH:9]=[N:27][CH:26]=[CH:12][CH:13]=3)[N:4]=2)[CH:24]=[CH:23][CH:22]=1
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참가 물질

4

반응물 3

HCID 13387N-methyl-2-pyrrolidoneHCID 22690363HCID 22690363, 화합물HCID 178503395HCID 178503395, 화합물

생성물 1

HCID 178521288HCID 178521288, 화합물수율 85%

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온도
140 °C

실험 절차

The sulfone from Step B (101 mg, 0.567 mmol) was dissolved in NMP (2 ml). To this solution 2-amino-N-(3-chlorophenyl)-acetamide (116 mg, 5 mmol) was added, and the mixture was heated at 140° C. for 12 h. The mixture was loaded directly onto an HPLC reverse phase column and purified by water to acetonitrile gradient in the presence of 0.1% trifluoroacetic acid. The aqueous phase was evaporated by lyophilization to yield the title compound as a fluffy white solid (166 mg, 85% yield). ES (MS): 345.12 (M+H)+

후처리

  1. custompurified by water to acetonitrile gradient in the presence of 0.1% trifluoroacetic acid
  2. customThe aqueous phase was evaporated by lyophilization

출처 및 근거

ORD 기록
ord-760e0727b39e4eab8f7a7c5ddd5878a4
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07361669B2

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