Carbon tetrabromide → HCID 22981310、化合物

HRID 1861961ノート

反応式

HRID 1861961 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 22981310HCID 22981310、化合物収率 36.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-4a27f0bff4a0406d827c1f1f587b975d
出典データセット
uspto-grants-2003_03
特許番号
US06534546B1

反応ノート

読み込み中…