1-Oxaspiro[5.5]undec-3-ene, 4-methyl- → HCID 3764775, 화합물

HRID 716484노트

반응식

HRID 716484 반응식
[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

참가 물질

5

반응물 2

HCID 111164241-Oxaspiro[5.5]undec-3-ene, 4-methyl-HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 3764775HCID 3764775, 화합물수율 93%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 3776Isopropanol용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-3a6a16655d5743fc9ca3d68d22cd5821
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187709B2

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