Carbon tetrabromide → HCID 22981310, 화합물

HRID 1861961노트

반응식

HRID 1861961 반응식
[C:1]([O:5][C:6](=[O:17])[NH:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14]O)=[CH:10][C:9]=1[CH3:16])([CH3:4])([CH3:3])[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Br)(Br)(Br)[Br:38]>C(Cl)Cl>[C:1]([O:5][C:6](=[O:17])[NH:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][Br:38])=[CH:10][C:9]=1[CH3:16])([CH3:4])([CH3:3])[CH3:2]

참가 물질

5

반응물 3

HCID 11205Carbon tetrabromideHCID 11776TriphenylphosphineHCID 22981315tert-butyl N-[4-(hydroxymethyl)-2-methylphenyl]carbamate

생성물 1

HCID 22981310HCID 22981310, 화합물수율 36.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The compound (1.035 g) obtained in Example 518 was dissolved in methylene chloride (20 ml) and to the solution, triphenylphosphine (1.38 g) and carbon tetrabromide (1.74 g) were successively added under ice cooling. The reaction mixture was stirred for 30 min under ice cooling, then stirred at room temperature for 30 min and the solvent was distilled off under reduced pressure. The resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=5:1) to give 476.6 mg of the titled compound (yield, 36%).

후처리

  1. additionwere successively added under ice cooling
  2. stirringstirred at room temperature for 30 min
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography (eluent, n-hexane:ethyl acetate=5:1)

출처 및 근거

ORD 기록
ord-4a27f0bff4a0406d827c1f1f587b975d
출처 데이터셋
uspto-grants-2003_03
특허 번호
US06534546B1

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