1-Oxaspiro[5.5]undec-3-ene, 4-methyl- → HCID 3764775、化合物

HRID 716491ノート

反応式

HRID 716491 の反応式
[CH3:1][C:2]1[CH2:7][C:6]2([CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)[O:5][CH2:4][CH:3]=1.[H][H]>[Ni].C(O)(C)C>[CH3:1][CH:2]1[CH2:7][C:6]2([CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)[O:5][CH2:4][CH2:3]1

参加物

5

反応物 2

HCID 111164241-Oxaspiro[5.5]undec-3-ene, 4-methyl-HCID 178418361HCID 178418361、化合物

生成物 1

HCID 3764775HCID 3764775、化合物収率 93%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 3776Isopropanol溶媒

実験手順

A solution of 4-methyl-1-oxaspiro[5.5]undec-3-ene (1.66 kg, 10.0 mols), isopropyl alcohol (100 ml) and Raney nickel (100 g) or other suitable sponge-metal catalyst was hydrogenated at 400 psi, at 140° C. for 10-12 h until the theoretical amount of hydrogen was taken up. The mixture was cooled and filtrated. The isopropyl alcohol was evaporated and the residue obtained was distilled under reduced pressure to provide 4-methyl-1-oxaspiro [5.5] undecane (1.56 kg, yield: 93%, purity: 99% sum of the isomers).

後処理

  1. temperatureThe mixture was cooled
  2. filtrationfiltrated
  3. customThe isopropyl alcohol was evaporated
  4. customthe residue obtained
  5. distillationwas distilled under reduced pressure

出典と根拠

ORDレコード
ord-ce2c954baa4f4245bddaef47eff299fb
出典データセット
uspto-grants-2015_11
特許番号
US09187709B2

反応ノート

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