Maleic Anhydride → 4-[(6-chloro-1H-indazol-3-yl)amino]-4-oxo-2-butenoic acid

HRID 497582

反応式

HRID 497582 の反応式
[C:1]1(=[O:7])[O:6][C:4](=[O:5])[CH:3]=[CH:2]1.[Cl:8][C:9]1[CH:17]=[C:16]2[C:12]([C:13]([NH2:18])=[N:14][NH:15]2)=[CH:11][CH:10]=1>C1(C)C(C)=CC=CC=1>[Cl:8][C:9]1[CH:17]=[C:16]2[C:12]([C:13]([NH:18][C:1](=[O:7])[CH:2]=[CH:3][C:4]([OH:6])=[O:5])=[N:14][NH:15]2)=[CH:11][CH:10]=1

参加物

4

反応物 2

HCID 7923Maleic AnhydrideHCID 856286-chloro-1H-indazol-3-amine

生成物 1

HCID 670427914-[(6-chloro-1H-indazol-3-yl)amino]-4-oxo-2-butenoic acid収率 63.1%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度
145 °C

実験手順

585 mg of preground maleic anhydride are added to 1 g of 6-chloro-1H-indazole-3-amine in 30 cm3 of ortho-xylene. The reaction medium is refluxed at 145° C. for ten minutes and then cooled in a water bath. The insoluble material is filtered off and washed successively with 2×25 cm3 of ethyl acetate and then with 2×25 cm3 of diisopropyl ether. The solid is then dried under reduced pressure (90 Pa; 50° C.) to give 1 g of 4-[(6-chloro-1H-indazol-3-yl)amino]-4-oxo-2-butenoic acid (Z form) in the form of yellow crystals melting at 230° C.

後処理

  1. temperaturecooled in a water bath
  2. filtrationThe insoluble material is filtered off
  3. washwashed successively with 2×25 cm3 of ethyl acetate
  4. customThe solid is then dried under reduced pressure (90 Pa; 50° C.)

出典と根拠

ORDレコード
ord-753497c62f804f97b114565b58b850c0
出典データセット
uspto-grants-2005_09
特許番号
US06949579B2

関連ノート

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