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Triethylamine → HCID 58142730, 화합물

HRID 1640338
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HRID 1640338 반응식
Cl/[C:2](=[N:8]\[NH:9][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[F:17])/[C:3]([O:5][CH2:6][CH3:7])=[O:4].CS[C:20]1[NH:24][N:23]=[CH:22][N:21]=1.C(N(CC)CC)C>O1CCOCC1>[F:17][C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][C:11]=1[CH2:10][N:9]1[C:22]2=[N:23][N:24]=[CH:20][N:21]2[C:2]([C:3]([O:5][CH2:6][CH3:7])=[O:4])=[N:8]1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 5753783-Methylthio-4H-1,2,4-triazoleHCID 58142732ethyl (2Z)-2-chloro-2-[(2-fluorophenyl)methylhydrazinylidene]acetate

생성물 1

HCID 58142730HCID 58142730, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

Ethyl(2Z)-chloro[(2-fluorobenzyl)hydrazono]acetate (807 mg, 3.12 mmol) from example 2A, 5-(methylthio)-1H-1,2,4-triazole (359 mg, 3.12 mmol) and triethylamine (316 mg, 3.12 mmol) are dissolved in dioxane (5 ml) and heated under reflux for 6 h. This is followed by dilution with water and extraction with ethyl acetate. The organic phase is dried over sodium sulfate, and the crude product is purified by chromatography on silica gel (eluent: dichloromethane/methanol 50:1). 124 mg (9.5% of theory) of the desired product are obtained with 69% purity.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 6 h
  3. extractionThis is followed by dilution with water and extraction with ethyl acetate
  4. dry with materialThe organic phase is dried over sodium sulfate
  5. customthe crude product is purified by chromatography on silica gel (eluent: dichloromethane/methanol 50:1)

출처 및 근거

ORD 기록
ord-ced263f4cd55478fb73a13234c96c764
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08114400B2

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