반응 #80142

반응 방정식

N-{7-[bis-(4-methyl-benzyl)-amino]-4-methoxy-benzothiazol-2-yl}-benzamide

2,2,2-trichloroethyl chloroformate

→

(2-benzoylamino-4-methoxy-benzothiazol-7-yl)-(4-methyl-benzyl)-carbamic acid 2,2,2-trichloro-ethyl ester

수율 40.4%

용매

acetonitrile

반응 조건

후처리

1. 1
   농축The mixture was then concentrated in vacuo

실험 절차

To a stirred solution of 300 mg (0.59 mmol) N-{7-[bis-(4-methyl-benzyl)-amino]-4-methoxy-benzothiazol-2-yl}-benzamide in 10 ml acetonitrile was added dropwise 0.60 ml (4.46 mmol) 2,2,2-trichloroethyl chloroformate and the reaction mixture heated at 80° C. for 72 h. The mixture was then concentrated in vacuo. Flash chromatography (ethyl acetate/hexane) afforded 138 mg (40%) (2-benzoylamino-4-methoxy-benzothiazol-7-yl)-(4-methyl-benzyl)-carbamic acid 2,2,2-trichloro-ethyl ester as a yellow solid. ES-MS m/e (%):584 (M{37Cl, 37Cl, 37Cl}+H+, 5), 582 (M{37Cl, 37Cl, 35Cl}+H+, 32), 580 (M{37Cl, 35Cl, 35Cl}+H+, 100), 578 (M{35Cl, 35Cl, 35Cl}+H+, 92).

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