Butanedione → 1-Adamantanol

HRID 2305273노트

반응식

HRID 2305273 반응식
[C:1]12([OH:11])[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.[C:12](C(C)=O)([CH3:14])=[O:13].O=O>C([O-])(=O)C.[Co+2].C([O-])(=O)C.C(O)(=O)C>[C:12]([C:3]12[CH2:4][CH:5]3[CH2:6][CH:7]([CH2:8][C:1]([OH:11])([CH2:10]3)[CH2:2]1)[CH2:9]2)(=[O:13])[CH3:14].[C:1]12([OH:11])[CH2:8][CH:7]3[CH2:6][CH:5]([CH2:4][CH:3]([CH2:9]3)[CH2:2]1)[CH2:10]2

참가 물질

7

반응물 3

HCID 650ButanedioneHCID 977OxygenHCID 641521-Adamantanol

생성물 2

HCID 641521-AdamantanolHCID 5918961-Acetyl-3-hydroxyadamantane

시약·촉매·용매 2

HCID 6277Cobalt diacetate촉매HCID 176Acetic Acid용매

실험 절차

A mixture of 0.3 mol of 1-adamantanol, 1.8 mol of biacetyl, 1.5 mmole of cobalt(II) acetate, and 300 ml of acetic acid was stirred at 60° C. in an oxygen atmosphere (1 atm) for 4 hours. The reaction mixture was concentrated to about 20% by weight, and was extracted with ethyl acetate, was dried, and was washed with hexane to yield 1-acetyl-3-adamantanol in a yield of 20% with a conversion rate from 1-adamantanol of 82%.

후처리

  1. concentrationThe reaction mixture was concentrated to about 20% by weight
  2. extractionwas extracted with ethyl acetate
  3. customwas dried
  4. washwas washed with hexane

출처 및 근거

ORD 기록
ord-fcd436595e854bf58e4a24909368b811
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06440636B1

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