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

HRID 18580

反応式

HRID 18580 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-d15e672edb1b49a3871841e558853d66
出典データセット
uspto-grants-2010_06
特許番号
US07741341B2

関連ノート

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