Morpholine → 4-Isopropenyl-1-methyl-2-morpholin-4-yl-cyclohexanol

HRID 1435599

반응식

HRID 1435599 반응식
[CH3:1][C:2]([CH:4]1[CH2:9][CH:8]2[O:10][C:7]2([CH3:11])[CH2:6][CH2:5]1)=[CH2:3].[Cl-].[Li+].[NH:14]1[CH2:19][CH2:18][O:17][CH2:16][CH2:15]1>C(O)C>[C:2]([CH:4]1[CH2:5][CH2:6][C:7]([CH3:11])([OH:10])[CH:8]([N:14]2[CH2:19][CH2:18][O:17][CH2:16][CH2:15]2)[CH2:9]1)([CH3:1])=[CH2:3]

참가 물질

5

반응물 3

HCID 8083MorpholineHCID 91496Limonene oxideHCID 433294Lithium Chloride

생성물 1

HCID 226252054-Isopropenyl-1-methyl-2-morpholin-4-yl-cyclohexanol수율 49.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

(+)-Limonene oxide (13.2 g, 0.087 moles) was dissolved in ethanol (40 ml) and lithium chloride (5.9 g, 0.14 moles) was added with stirring. Morpholine (11.4 g, 0.13 moles) was added and the reaction mixture was heated at 60° for 48 hours. The solvent was evaporated under reduced pressure and the residue taken up in dichloromethane. Washed with water. Extracted into 2M hydrochloric acid and washed with dichloromethane. Basified to pH 10 by addition of 2M sodium hydroxide. Extracted with diethyl ether and washed with water. Dried over anhydrous magnesium sulphate and evaporated the solvent under reduced pressure to give the product as a yellow oil (10.3 g)

후처리

  1. temperaturethe reaction mixture was heated at 60° for 48 hours
  2. customThe solvent was evaporated under reduced pressure
  3. washWashed with water
  4. extractionExtracted into 2M hydrochloric acid
  5. washwashed with dichloromethane
  6. additionBasified to pH 10 by addition of 2M sodium hydroxide
  7. extractionExtracted with diethyl ether
  8. washwashed with water
  9. dry with materialDried over anhydrous magnesium sulphate
  10. customevaporated the solvent under reduced pressure

출처 및 근거

ORD 기록
ord-dcf5863657d44a41b00edbbd6568b851
출처 데이터셋
uspto-grants-2009_11
특허 번호
US07618966B2

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