Sodium Hydroxide → HCID 68469685、化合物

HRID 387653ノート

反応式

HRID 387653 の反応式
[CH3:1][N:2]([S:25]([CH3:28])(=[O:27])=[O:26])[C:3]1[CH:4]=[C:5]([C:21]([O:23]C)=[O:22])[C:6]2[CH2:7][CH2:8][N:9]([CH:14]([CH2:18][CH2:19][CH3:20])[CH2:15][CH2:16][CH3:17])[C:10](=[O:13])[C:11]=2[CH:12]=1.[OH-].[Na+]>O1CCOCC1>[CH3:1][N:2]([S:25]([CH3:28])(=[O:26])=[O:27])[C:3]1[CH:4]=[C:5]([C:21]([OH:23])=[O:22])[C:6]2[CH2:7][CH2:8][N:9]([CH:14]([CH2:18][CH2:19][CH3:20])[CH2:15][CH2:16][CH3:17])[C:10](=[O:13])[C:11]=2[CH:12]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 68474347HCID 68474347、化合物

生成物 1

HCID 68469685HCID 68469685、化合物収率 96.5%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

0.25 g of methyl 7-[methyl(methylsulfonyl)amino]-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxylate is dissolved in 5 cm3 of dioxane at a temperature close to 20° C. 1.52 cm3 of a 1M aqueous solution of sodium hydroxide are added, then the reaction mixture is heated at a temperature close to 60° C. for 1 h. The dioxane contained in the reaction mixture is concentrated using a rotary evaporator under reduced pressure (5 kPa). 20 cm3 of ethyl ether and 10 cm3 of water are added to the residue obtained. After decanting, the aqueous phase is acidified with 1.6 cm3 of a 1M aqueous solution of hydrochloric acid. The aqueous phase is extracted with 20 cm3 of dichloromethane. After decanting, the organic phase is dried over magnesium sulfate, filtered then concentrated using a rotary evaporator under reduced pressure (5 kPa). 0.233 g of 7-[methyl(methylsulfonyl)amino]-1-oxo-2-(1-propylbutyl)-1,2,3,4-tetrahydroisoquinoline-5-carboxylic acid is obtained in the form of a pale pink powder.

後処理

  1. customclose to 20° C
  2. temperaturethe reaction mixture is heated at a temperature
  3. customclose to 60° C. for 1 h
  4. concentrationis concentrated
  5. customa rotary evaporator under reduced pressure (5 kPa)
  6. addition20 cm3 of ethyl ether and 10 cm3 of water are added to the residue
  7. customobtained
  8. customAfter decanting
  9. extractionThe aqueous phase is extracted with 20 cm3 of dichloromethane
  10. customAfter decanting
  11. dry with materialthe organic phase is dried over magnesium sulfate
  12. filtrationfiltered
  13. concentrationthen concentrated
  14. customa rotary evaporator under reduced pressure (5 kPa)

出典と根拠

ORDレコード
ord-e33ccca63d5b4bd3ab2efcd8bb72f1b5
出典データセット
uspto-grants-2013_02
特許番号
US08372864B2

反応ノート

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