Methyl chloroformate → HCID 13575671, 화합물

HRID 465023노트

반응식

HRID 465023 반응식
[CH3:1][CH:2]1[CH2:6][C:5]2[C:7]([CH3:13])=[CH:8][CH:9]=[C:10]([NH:11][NH2:12])[C:4]=2[O:3]1.C(N(CC)C(C)C)(C)C.Cl[C:24]([O:26][CH3:27])=[O:25]>C1COCC1>[CH3:27][O:26][C:24]([NH:12][NH:11][C:10]1[C:4]2[O:3][CH:2]([CH3:1])[CH2:6][C:5]=2[C:7]([CH3:13])=[CH:8][CH:9]=1)=[O:25]

참가 물질

5

반응물 3

HCID 6586Methyl chloroformateHCID 81531DiisopropylethylamineHCID 13575670HCID 13575670, 화합물

생성물 1

HCID 13575671HCID 13575671, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
-5 °C

실험 절차

15.6 g of 1E was mixed with 150 ml of THF and 11.3 g of N,N-diisopropylethylamine. The mixture was cooled to -5° C. and 9.1 g of methyl chloroformate was added drop-by-drop to the stirred mixture, stirred at 0° C. for two hours, then poured over ice water and extracted with ether. The extract was dried (MgSO4) and the solvent was evaporated. The residue was column chromatographed on silica gel, using a 1:4:20 v:v:v mixture of tetrahydrofuran, ethyl acetate and hexane as eluent, to give 2-(2,3-dihydro-2,4-dimethylbenzofuran-7-yl)hydrazinecarboxylic acid methyl ester (1F), as a tan solid, m.p.: 90°-92° C.

후처리

  1. extractionextracted with ether
  2. dry with materialThe extract was dried (MgSO4)
  3. customthe solvent was evaporated
  4. customchromatographed on silica gel
  5. additionv:v mixture of tetrahydrofuran, ethyl acetate and hexane as eluent

출처 및 근거

ORD 기록
ord-0e30df148e214556a028d39347442c01
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04550121

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