Benzyl Alcohol → HCID 11735856, 화합물

HRID 1683385

반응식

HRID 1683385 반응식
[CH2:1]([OH:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.N1C=CC=CC=1.[CH3:15][CH:16]([CH2:20][CH:21]=[CH2:22])[C:17](Cl)=[O:18]>CN(C)C1C=CN=CC=1.C(Cl)Cl>[C:2]1([CH2:1][O:8][C:17](=[O:18])[CH:16]([CH3:15])[CH2:20][CH:21]=[CH2:22])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 244Benzyl AlcoholHCID 1049PyridineHCID 129214422-Methyl-4-pentenoyl chloride

생성물 1

HCID 11735856HCID 11735856, 화합물수율 78.3%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매2회

실험 절차

To a 0° C. solution of 23.8 g of benzyl alcohol, 0.05 g of 4-(dimethylamino)pyridine, 18.3 g of pyridine and 250 ml of methylene chloride is added, dropwise, a solution of 29.5 g of racemic 2-methyl-4-pentenoyl chloride in 50 ml of methylene chloride. The mixture is stirred at room temperature for 4 hours, followed by successive washing with 2N hydrochloric acid, saturated sodium bicarbonate and saturated sodium chloride. The organic layer is dried and concentrated in vacuo. The residue is purified by Kugelrohr distillation to give 35.2 g of the desired product as a colorless oil; bp 70°-75° C. at 0.10 mm Hg.

후처리

  1. washby successive washing with 2N hydrochloric acid, saturated sodium bicarbonate and saturated sodium chloride
  2. customThe organic layer is dried
  3. concentrationconcentrated in vacuo
  4. distillationThe residue is purified by Kugelrohr distillation

출처 및 근거

ORD 기록
ord-ac753da4b3714b3a886a2d6d3a89404d
출처 데이터셋
uspto-grants-1997_06
특허 번호
US05637731

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