Water → HCID 18800826, 화합물

HRID 849140

반응식

HRID 849140 반응식
N1([C:6]2[CH2:11][CH2:10][CH2:9][CH2:8][CH:7]=2)CCCC1.O=C1CCCCC1[CH:19]([CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)[C:20]([O:22]C)=[O:21].[OH2:31].[Li+].[OH-].[CH3:34]O>CN(C)C=O>[O:31]=[C:26]1[CH2:27][CH2:28][CH2:29][CH2:30][CH:25]1[CH:24]([C:6]1[CH:7]=[CH:8][C:9]([CH3:34])=[CH:10][CH:11]=1)[CH2:19][C:20]([OH:22])=[O:21]

참가 물질

6

반응물 4

HCID 962WaterHCID 707681-Pyrrolidino-1-cyclohexeneHCID 13268645HCID 13268645, 화합물HCID 23717829Lithium hydroxide methanol

생성물 1

HCID 18800826HCID 18800826, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1-pyrrolidino-1-cyclohexene is refluxed with methyl a-(2-oxocyclohexyl)benzenepropanoate in dimethylformamide (DMF) for 24 hours and refluxing is continued for another hour after the addition of water. DMF is removed under reduced pressure and the residue is diluted with water and extracted three times with EtOAc. The combined EtOAc extracts are washed with 1N HCl and then with brine. The organic phase is dried over MgSO4 and evaporated to give crude methyl b-(2-cxocyclohexyl)-4-methylbenzenepropanoate. This material is treated with 1 N LiOH/methanol to give the title material.

후처리

  1. temperaturerefluxing
  2. waitis continued for another hour
  3. customDMF is removed under reduced pressure
  4. additionthe residue is diluted with water
  5. extractionextracted three times with EtOAc
  6. washThe combined EtOAc extracts are washed with 1N HCl
  7. dry with materialThe organic phase is dried over MgSO4
  8. customevaporated
  9. customto give crude methyl b-(2-cxocyclohexyl)-4-methylbenzenepropanoate

출처 및 근거

ORD 기록
ord-65f23ca2dfcd4464b30fa58930cbe4ac
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06011028

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