Trifluoroacetic acid → n-(4-Amino-3-methylphenyl) {[(5-chloro(2-thienyl))sulfonyl]amino}-carboxamide

HRID 1828139ノート

反応式

HRID 1828139 の反応式
C(OC([NH:8][C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16]([NH:18][S:19]([C:22]2[S:23][C:24]([Cl:27])=[CH:25][CH:26]=2)(=[O:21])=[O:20])=[O:17])=[CH:11][C:10]=1[CH3:28])=O)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:8][C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16]([NH:18][S:19]([C:22]2[S:23][C:24]([Cl:27])=[CH:25][CH:26]=2)(=[O:21])=[O:20])=[O:17])=[CH:11][C:10]=1[CH3:28]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 22064442N-(4-[(tert-butoxy)carbonylamino]-3-methylphenyl}{[(5-chloro(2-thienyl))sulfonyl]amino}carboxamide

生成物 1

HCID 22064409n-(4-Amino-3-methylphenyl) {[(5-chloro(2-thienyl))sulfonyl]amino}-carboxamide収率 136.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a chilled solution of N-{4-[(tert-butoxy)carbonylamino]-3-methylphenyl}{[(5-chloro(2-thienyl))sulfonyl]amino}carboxamide (0.246 g, 0.55 mmol) in CH2Cl2 (5 mL) was added neat TFA (1.1 mL). The reaction mixture was stirred cold for 1.5 hr, concentrated in vacuo, azeotroped with heptane and dried to give N-(4-amino-3-methylphenyl) {[(5-chloro(2-thienyl))sulfonyl]amino}-carboxamide (0.26 g) as the mono TFA salt. ES-MS (M+H)+=346.

後処理

  1. concentrationconcentrated in vacuo
  2. customazeotroped with heptane
  3. customdried

出典と根拠

ORDレコード
ord-da9fe9cdf5784a39881d29965b8f67c3
出典データセット
uspto-grants-2006_06
特許番号
US07056926B2

反応ノート

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