Water → 4-{[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-amino}-3-nitro-benzoic acid methyl ester

HRID 18580

반응식

HRID 18580 반응식
[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[CH:8][C:7](F)=[C:6]([N+:11]([O-:13])=[O:12])[CH:5]=1.[Cl:15][C:16]1[S:20][C:19]([C:21]2[O:25][N:24]=[C:23]([CH2:26][NH2:27])[CH:22]=2)=[CH:18][CH:17]=1.C(N(CC)CC)C.O>CN(C=O)C>[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[CH:8][C:7]([NH:27][CH2:26][C:23]2[CH:22]=[C:21]([C:19]3[S:20][C:16]([Cl:15])=[CH:17][CH:18]=3)[O:25][N:24]=2)=[C:6]([N+:11]([O-:13])=[O:12])[CH:5]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 5219721Methyl 4-fluoro-3-nitrobenzoateHCID 68616593(5-(5-Chlorothiophen-2-yl)isoxazol-3-yl)methanamine

생성물 1

HCID 686158574-{[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-ylmethyl]-amino}-3-nitro-benzoic acid methyl ester

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 634.4 mg (3.19 mmol) 4-Fluoro-3-nitro-benzoic acid methyl ester in 12 mL DMF were added 800.0 mg (3.19 mmol) C-[5-(5-Chloro-thiophen-2-yl)-isoxazol-3-yl]-methylamine and 0.88 mL (6.37 mmol) triethylamine. The reaction mixture was stirred at room temperature for 16 h. 12 mL water was added. The precipitate was filtered off and washed with water. The yellow crystalline material was dried under reduced pressure at 40° C.

후처리

  1. filtrationThe precipitate was filtered off
  2. washwashed with water
  3. customThe yellow crystalline material was dried under reduced pressure at 40° C.

출처 및 근거

ORD 기록
ord-d15e672edb1b49a3871841e558853d66
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07741341B2

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