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1,3-Dichloroacetone → HCID 68503221, 화합물

HRID 1710776
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인쇄 미리보기

반응식

HRID 1710776 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:14]=[CH:13][C:9]([C:10]([NH2:12])=[O:11])=[C:8]([F:15])[CH:7]=1.[Cl:16][CH2:17][C:18]([CH2:20]Cl)=O>C(#N)CC>[Cl:16][CH2:17][C:18]1[N:12]=[C:10]([C:9]2[CH:13]=[CH:14][C:6]([O:5][CH2:4][CH2:3][CH2:2][Cl:1])=[CH:7][C:8]=2[F:15])[O:11][CH:20]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 107931,3-DichloroacetoneHCID 59457468HCID 59457468, 화합물

생성물 1

HCID 68503221HCID 68503221, 화합물수율 44%

시약·촉매·용매 1

HCID 7854Propionitrile용매

반응 조건

온도
100 °C

실험 절차

A mixture of 4-(3-chloropropoxy)-2-fluorobenzamide i82 (0.41 g, 1.75 mmol, 1 eq) and 1,3-dichloroacetone (0.49 g, 3.85 mmol, 2.2 eq) in propionitrile (9 ml) is stirred at 100° C. for 60 h. The mixture is then concentrated under vacuum, taken up in dichloromethane, and washed with water. The organic phase is dried over magnesium sulfate and concentrated under reduced pressure. The residue is purified by chromatography over silicagel (eluent: dichloromethane) to afford 0.23 g of 4-(chloromethyl)-2-[4-(3-chloropropoxy)-2-fluorophenyl]-1,3-oxazole i84.

후처리

  1. concentrationThe mixture is then concentrated under vacuum
  2. washwashed with water
  3. dry with materialThe organic phase is dried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue is purified by chromatography over silicagel (eluent: dichloromethane)

출처 및 근거

ORD 기록
ord-27f1f66004f9426986bd62f9d4852ae5
출처 데이터셋
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07790720B2

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