HCID 23325917、化合物 → Bicyclo[3.2.1]octan-8-ol, 8-ethyl-1,5-dimethyl-

HRID 1380712ノート

反応式

HRID 1380712 の反応式
[CH3:1][C:2]12[C:9]([C:11]#[CH:12])([OH:10])[C:6]([CH3:13])([CH2:7][CH2:8]1)[CH2:5][CH2:4][CH2:3]2.[H][H]>[Ni]>[CH3:13][C:6]12[C:9]([CH2:11][CH3:12])([OH:10])[C:2]([CH3:1])([CH2:8][CH2:7]1)[CH2:3][CH2:4][CH2:5]2

参加物

4

反応物 2

HCID 23325917HCID 23325917、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 163418Bicyclo[3.2.1]octan-8-ol, 8-ethyl-1,5-dimethyl-収率 85%

試薬・触媒・溶媒 1

HCID 935Nickel触媒

実験手順

A solution of 178 g (1 mole) 5 in 1000 ml destilled methanole was mixed with 1 g Raney nickel and hydrogenated in an autoclave (20 bar/20° to 30° C.). After about 4 h the uptake of hydrogen was finished (2 equivalents H2). The reaction mixture was taken from the autoclave, filtered, evaporated and distilled. This resulted in 155 g (85%) of 7 in form of a colorless oil having a boiling point (1 mm) of 68° C. IR: 3500/3600 cm-1 (O--H).--NMR (CCl4): δ=0.88, s (1-, 5-CH2), 0.97, t, J=7 Hz (--CH2 --CH3), 1.45 ppm, br.s (6-, 7-CH2).--MS: m/e (%)=153 (100, M+ -29), 135 (56), 125 (20), 123 (20), 107 (71), 99 (20), 95 (45), 69 (46).C12H22O (M=182.30).

後処理

  1. customhydrogenated in an autoclave (20 bar/20° to 30° C.)
  2. filtrationfiltered
  3. customevaporated
  4. distillationdistilled

出典と根拠

ORDレコード
ord-8028835653f240d48959d6a7019f4be5
出典データセット
uspto-grants-1986_04
特許番号
US04582945

反応ノート

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