Water → HCID 18800826、化合物

HRID 849140

反応式

HRID 849140 の反応式
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]

参加物

6

反応物 4

HCID 962WaterHCID 707681-Pyrrolidino-1-cyclohexeneHCID 13268645HCID 13268645、化合物HCID 23717829Lithium hydroxide methanol

生成物 1

HCID 18800826HCID 18800826、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-65f23ca2dfcd4464b30fa58930cbe4ac
出典データセット
uspto-grants-2000_01
特許番号
US06011028

関連ノート

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