Sodium Hydroxide → HCID 68473089, 화합물

HRID 387680노트

반응식

HRID 387680 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([C:20]([O:22]C)=[O:21])[C:5]2[CH2:6][CH2:7][N:8]([CH:13]([CH2:17][CH2:18][CH3:19])[CH2:14][CH2:15][CH3:16])[C:9](=[O:12])[C:10]=2[CH:11]=1.[OH-].[Na+]>O1CCOCC1>[CH3:1][C:2]1[CH:3]=[C:4]([C:20]([OH:22])=[O:21])[C:5]2[CH2:6][CH2:7][N:8]([CH:13]([CH2:14][CH2:15][CH3:16])[CH2:17][CH2:18][CH3:19])[C:9](=[O:12])[C:10]=2[CH:11]=1

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 68469403HCID 68469403, 화합물

생성물 1

HCID 68473089HCID 68473089, 화합물수율 106.2%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

33 mg of methyl 7-methyl-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxylate are dissolved in 1 cm3 of dioxane at a temperature close to 20° C. 0.3 cm3 of a 1N aqueous solution of sodium hydroxide is added, then the reaction mixture is heated at a temperature close to 60° C. for 1 h. The mixture is then concentrated to dryness under reduced pressure (5 kPa), taken up by 10 cm3 of water and 15 cm3 of ethyl ether. The aqueous phase is decanted, washed with 10 cm3 of ethyl ether, acidified with 0.3 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). 33.5 mg of 7-methyl-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxylic acid are obtained in the form of a colorless lacquer.

후처리

  1. customclose to 20° C
  2. temperaturethe reaction mixture is heated at a temperature
  3. customclose to 60° C. for 1 h
  4. concentrationThe mixture is then concentrated to dryness under reduced pressure (5 kPa)
  5. customThe aqueous phase is decanted
  6. washwashed with 10 cm3 of ethyl ether
  7. extractionThe organic phase is extracted
  8. dry with materialdried over anhydrous magnesium sulfate
  9. filtrationfiltered
  10. concentrationconcentrated to dryness under reduced pressure (5 kPa)

출처 및 근거

ORD 기록
ord-3ec256772cae46ceba3d17df1123b3da
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372864B2

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