Ethanol → 1-benzhydrylazetidine-2-carboxylic Acid

HRID 1731238노트

반응식

HRID 1731238 반응식
[CH:1]([N:14]1CC[CH:15]1[CH2:18]C#N)([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[OH-:21].[Na+].[CH2:23]([OH:25])[CH3:24]>O>[CH:1]([N:14]1[CH2:15][CH2:18][CH:24]1[C:23]([OH:21])=[O:25])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 20228404[1-(Diphenylmethyl)azetidin-2-yl]acetonitrile

생성물 1

HCID 99034621-benzhydrylazetidine-2-carboxylic Acid

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

A mixture of the 1C, 2.5 g of sodium hydroxide, 36 ml of ethanol and 24 ml of water was refluxed for 6 hours, then left to cool for 16 hours. The mixture then was poured into water, washed with ether and acidified to pH 5. The solvent was evaporated, the residue was taken up in methanol, the solution was filtered and the methanol was evaporated. The residue was dissolved in chloroform; the solution was washed with brine, dried and the solvent was evaporated, to give 1-benzhydryl-2-azetidine carboxylic acid (1D).

후처리

  1. temperaturewas refluxed for 6 hours
  2. waitleft
  3. temperatureto cool for 16 hours
  4. washwashed with ether
  5. customThe solvent was evaporated
  6. filtrationthe solution was filtered
  7. customthe methanol was evaporated
  8. dissolutionThe residue was dissolved in chloroform
  9. washthe solution was washed with brine
  10. customdried
  11. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-738cfb26eb8947e2afcca800debad3d6
출처 데이터셋
uspto-grants-1986_11
특허 번호
US04620866

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