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Diisopropylethylamine → HCID 44203076, 화합물

HRID 77369
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HRID 77369 반응식
[NH2:1][CH2:2][C:3]([NH:5][CH:6]([CH3:8])[CH3:7])=[O:4].C(N(CC)C(C)C)(C)C.[F:18][C:19]1[CH:20]=[CH:21][C:22]([N+:28]([O-:30])=[O:29])=[C:23]([CH:27]=1)[C:24](Cl)=[O:25]>ClCCl>[F:18][C:19]1[CH:20]=[CH:21][C:22]([N+:28]([O-:30])=[O:29])=[C:23]([CH:27]=1)[C:24]([NH:1][CH2:2][C:3]([NH:5][CH:6]([CH3:8])[CH3:7])=[O:4])=[O:25]
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참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 5338492-Amino-N-isopropylacetamideHCID 156548685-Fluoro-2-nitrobenzoyl chloride

생성물 1

HCID 44203076HCID 44203076, 화합물수율 80.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 2-amino-N-isopropylacetamide (11.3 g, 97.0 mmol) and N,N-diisopropylethylamine (20.1 g, 162 mmol) in dichloromethane (200 mL) was cooled using an ice water bath. A solution of 5-fluoro-2-nitrobenzoyl chloride (16.5 g, 81.0 mmol) in dichloromethane (200 mL) was added dropwise over 15 minutes. The resulting solution was stirred overnight. The reaction mixture was washed with 2N HCl solution (2×250 mL), brine (250 mL) and then dried over magnesium sulphate. The solution was filtered before concentrating under reduced pressure to afford 5-fluoro-N-(2-(isopropylamino)-2-oxoethyl)-2-nitrobenzamide (18.5 g, 65.0 mmol).

후처리

  1. washThe reaction mixture was washed with 2N HCl solution (2×250 mL), brine (250 mL)
  2. dry with materialdried over magnesium sulphate
  3. filtrationThe solution was filtered
  4. concentrationbefore concentrating under reduced pressure

출처 및 근거

ORD 기록
ord-e36acb5a9442418b8149bd6620d8e734
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08841289B2

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