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1,1'-Carbonyldiimidazole → HCID 22049200, 화합물

HRID 1832159
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HRID 1832159 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:9]([NH2:14])[C:10]([CH3:13])([OH:12])[CH3:11])[CH:5]=[CH:6][C:7]=1[F:8].[C:15](N1C=CN=C1)(N1C=CN=C1)=[O:16]>ClCCl>[F:1][C:2]1[CH:3]=[C:4]([CH:9]2[C:10]([CH3:11])([CH3:13])[O:12][C:15](=[O:16])[NH:14]2)[CH:5]=[CH:6][C:7]=1[F:8]
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참가 물질

4

반응물 2

HCID 682631,1'-CarbonyldiimidazoleHCID 18623229(+)-β-Amino-3,4-difluoro-α,α-dimethylbenzeneethanol

생성물 1

HCID 22049200HCID 22049200, 화합물수율 50%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A mixture of 1-(3,4-difluorophenyl)-2-methyl-2-hydroxypropylamine (3.00 g, 14.9 mmol) and carbonyldiimidazole (2.418 g, 14.9 mmol) in dichloromethane (150 mL) was heated at reflux temperature for 36 h and the solvent evaporated. The residue was purified by column chromatography on silica gel using chloroform/ethyl acetate (9:1) to give the product as a viscous oil which solidified on standing (1.80 g, 50% yield). The product was used in the next step without further characterization.

후처리

  1. temperaturewas heated
  2. temperatureat reflux temperature for 36 h
  3. customthe solvent evaporated
  4. customThe residue was purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-e8ff5e32a0f24432931efe60a52d3374
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07067534B1

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