Water → Methyl 4-hydrazinocarbonothioylamino-2-nitrobenzoate

HRID 2103819

반응식

HRID 2103819 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([N:11]=[C:12]=[S:13])=[CH:7][C:6]=1[N+:14]([O-:16])=[O:15])=[O:4].O.[NH2:18][NH2:19].O>O1CCCC1>[NH:18]([C:12]([NH:11][C:8]1[CH:9]=[CH:10][C:5]([C:3]([O:2][CH3:1])=[O:4])=[C:6]([N+:14]([O-:16])=[O:15])[CH:7]=1)=[S:13])[NH2:19]

참가 물질

5

반응물 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 860145914-Methoxycarbonyl-3-nitrophenyl isothiocyanate

생성물 1

HCID 86014590Methyl 4-hydrazinocarbonothioylamino-2-nitrobenzoate수율 85%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

A solution of the above synthesized 4-methoxycarbonyl-3-nitrophenyl isothiocyanate (149 mg, 0.62 mmol) in tetrahydrofuran (2.2 ml) was added dropwise to a solution of hydrazine monohydrate (94 mg, 1.87 mmol) in tetrahydrofuran (4.0 ml) at 000 over 20 minutes. After stirring at 0° C. for further 40 minutes, water was added, and the precipitated solid was filtered to obtain 142 mg of the desired product as a colorless solid (yield 85%).

후처리

  1. filtrationthe precipitated solid was filtered

출처 및 근거

ORD 기록
ord-cb4f7a46d0c4472997f7a828bd10ed3a
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07576115B2

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