Sodium Hydroxide → HCID 68471625, 화합물

HRID 387676노트

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HRID 387676 반응식
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[CH:10]=[C:11]([C:27]([O:29]C)=[O:28])[C:12]2[CH2:13][CH2:14][N:15]([CH:20]([CH2:24][CH2:25][CH3:26])[CH2:21][CH2:22][CH3:23])[C:16](=[O:19])[C:17]=2[CH:18]=1)#[N:2].[OH-].[Na+]>O1CCOCC1>[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[C:9]1[CH:10]=[C:11]([C:27]([OH:29])=[O:28])[C:12]2[CH2:13][CH2:14][N:15]([CH:20]([CH2:21][CH2:22][CH3:23])[CH2:24][CH2:25][CH3:26])[C:16](=[O:19])[C:17]=2[CH:18]=1)#[N:2]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 68473665HCID 68473665, 화합물

생성물 1

HCID 68471625HCID 68471625, 화합물수율 99.5%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

178 mg of methyl 7-(2-cyanophenyl)-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxylate are dissolved in 3.6 cm3 of dioxane at a temperature close to 20° C. 1.1 cm3 of a 1N aqueous solution of sodium hydroxide are added, then the reaction mixture is heated at a temperature close to 60° C. for 30 min. The mixture is then concentrated to dryness under reduced pressure (5 kPa), taken up by 20 cm3 of water and 20 cm3 of ethyl ether. The aqueous phase is washed with 5 cm3 of ethyl ether, acidified with 2 cm3 of a 2N aqueous solution of hydrochloric acid and taken up with 10 cm3 of dichloromethane. The organic phase is extracted, dried over anhydrous magnesium sulfate, filtered and concentrated to dryness under reduced pressure (5 kPa). 171 mg of 7-(2-cyanophenyl)-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxylic acid are obtained in the form of a white foam.

후처리

  1. customclose to 20° C
  2. temperaturethe reaction mixture is heated at a temperature
  3. customclose to 60° C. for 30 min
  4. concentrationThe mixture is then concentrated to dryness under reduced pressure (5 kPa)
  5. washThe aqueous phase is washed with 5 cm3 of ethyl ether
  6. extractionThe organic phase is extracted
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated to dryness under reduced pressure (5 kPa)

출처 및 근거

ORD 기록
ord-7c4f0bea07244494aa62a67c588124d3
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372864B2

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