Water → 2-[2-(Methylthioethoxy)-phenyl]-hydrazinecarboxylic acid methyl ester

HRID 4244

반응식

HRID 4244 반응식
[CH3:1][O:2][C:3](Cl)=[O:4].[CH3:6][S:7][CH2:8][CH2:9][O:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[NH:17][NH2:18].O>O1CCCC1.C(N(C(C)C)C(C)C)C>[CH3:1][O:2][C:3]([NH:18][NH:17][C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=1[O:10][CH2:9][CH2:8][S:7][CH3:6])=[O:4]

참가 물질

6

반응물 3

HCID 962WaterHCID 6586Methyl chloroformateHCID 542892902-(2-Methylthioethoxy)-phenylhydrazine

생성물 1

HCID 538333612-[2-(Methylthioethoxy)-phenyl]-hydrazinecarboxylic acid methyl ester

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 81531Diisopropylethylamine용매

반응 조건

온도
20 °C

실험 절차

5.6 ml of chloroformic acid methyl ester are added dropwise at 0° C. to 14.4 g of 2-(2-methylthioethoxy)-phenylhydrazine in 100 ml of tetrahydrofuran and 14 g of N-ethyldiisopropylamine. The reaction mixture is stirred at 20° C. for 2 hours; H2O is then added, and the mixture is repeatedly extracted with ethyl acetate. After customary further processing, a solid is obtained, and this is recrystallised from alcohol to thus yield the compond of the formula ##STR62## having a melting point of 92°-94° C.

후처리

  1. extractionthe mixture is repeatedly extracted with ethyl acetate
  2. customAfter customary further processing, a solid is obtained
  3. customthis is recrystallised from alcohol
  4. customto thus yield the compond of the formula

출처 및 근거

ORD 기록
ord-e8648a916c7c4fcfb8175365162e18a3
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725302

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