Hydrochloric Acid → Ammonia

HRID 1988925ノート

反応式

HRID 1988925 の反応式
[CH:1]1([NH:4][C:5]([C:7]2[CH:8]=[CH:9][C:10]([CH3:35])=[C:11]([C:13]3[CH:34]=[CH:33][C:16]4[C:17]([N:20]5[CH2:25][CH2:24][N:23](C(OC(C)(C)C)=O)[CH2:22][CH2:21]5)=[N:18][O:19][C:15]=4[CH:14]=3)[CH:12]=2)=[O:6])[CH2:3][CH2:2]1.Cl>CO.O1CCOCC1>[NH3:4].[CH:1]1([NH:4][C:5](=[O:6])[C:7]2[CH:8]=[CH:9][C:10]([CH3:35])=[C:11]([C:13]3[CH:34]=[CH:33][C:16]4[C:17]([N:20]5[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]5)=[N:18][O:19][C:15]=4[CH:14]=3)[CH:12]=2)[CH2:2][CH2:3]1

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 586564681,1-Dimethylethyl 4-(6-{5-[(cyclopropylamino)carbonyl]-2-methylphenyl}-1,2-benzisoxazol-3-yl)-1-piperazinecarboxylate2 回

生成物 2

HCID 222AmmoniaHCID 10045079N-Cyclopropyl-4-methyl-3-[3-(1-piperazinyl)-1,2-benzisoxazol-6-yl]benzamide

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of 1,1-dimethylethyl 4-(6-{5-[(cyclopropylamino)carbonyl]-2methylphenyl}-1,2-benzisoxazol-3-yl)-1-piperazinecarboxylate (Intermediate 26) in methanol (1 ml) was treated with a solution of hydrogen chloride in dioxan (4N, 1 ml) then stirred at room temp. for 18 h. The solvent was evaporated and the residue was re-dissolved in methanol and applied to an SCX cartridge (1 g). Elution with methanol followed by methanol:0.88 ammonia (99:1) gave the title compound as a white solid (0.016 g).

後処理

  1. customThe solvent was evaporated
  2. dissolutionthe residue was re-dissolved in methanol
  3. washElution with methanol

出典と根拠

ORDレコード
ord-2ce5580b1c7a4e349ae14181ef5dc6f1
出典データセット
uspto-grants-2010_01
特許番号
US07642276B2

反応ノート

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