HCID 12923297、化合物 → HCID 12923329、化合物

HRID 972060ノート

反応式

HRID 972060 の反応式
[C:1]([O:5][CH2:6][C@H:7]([CH3:19])[CH2:8]/[CH:9]=[CH:10]/[C@H:11]([CH3:18])[CH2:12][C:13]([O:15][CH2:16][CH3:17])=[O:14])([CH3:4])([CH3:3])[CH3:2].[H][H]>[Ni].C(OCC)(=O)C>[CH2:16]([O:15][C:13](=[O:14])[CH2:12][C@@H:11]([CH3:18])[CH2:10][CH2:9][CH2:8][C@@H:7]([CH3:19])[CH2:6][O:5][C:1]([CH3:4])([CH3:3])[CH3:2])[CH3:17]

参加物

5

反応物 2

HCID 12923297HCID 12923297、化合物HCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 12923329HCID 12923329、化合物

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 1.104 g. (4.084 mmoles) of (3R,7R)-E-Ethyl 8tert. butoxy-3,7-dimethyl-4-octenoate, a small amount of Raney nickel, and 30 ml of ethyl acetate was stirred in an atmosphere of hydrogen, at room temperature, for 2 hours during which time approximately one equivalent of hydrogen was taken up. The catalyst was filtered off and washed with ethyl acetate. Concentration of the combined filtrate and washes in vacuo followed by evaporative distillation afforded 1.045 g. (95%) of saturated ester (3S,7R)-Ethyl 8-tert. butoxy-3,7-dimethyloctanoate as a colorless oil, b.p. 80°-83° C. (bath temperature) (0.15 mm Hg.).

後処理

  1. additionA mixture of 1.104 g
  2. filtrationThe catalyst was filtered off
  3. washwashed with ethyl acetate
  4. distillationConcentration of the combined filtrate and washes in vacuo followed by evaporative distillation
  5. customafforded 1.045 g

出典と根拠

ORDレコード
ord-58259f18add541f3944917adfc147184
出典データセット
uspto-grants-1979_07
特許番号
US04163021

反応ノート

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