Acetic Anhydride → HCID 12838038、化合物

HRID 327402ノート

反応式

HRID 327402 の反応式
Cl.[Cl:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]2[C:12]=1[CH2:11][NH:10][CH2:9][CH2:8]2.[OH-].[Na+].C([O-])(O)=O.[Na+].[C:20](OC(=O)C)(=[O:22])[CH3:21]>ClCCl>[C:20]([N:10]1[CH2:9][CH2:8][C:7]2[C:12](=[C:3]([Cl:2])[CH:4]=[CH:5][CH:6]=2)[CH2:11]1)(=[O:22])[CH3:21]

参加物

6

反応物 4

HCID 7918Acetic AnhydrideHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 125950728-Chloro-1,2,3,4-tetrahydroisoquinoline hydrochloride

生成物 1

HCID 12838038HCID 12838038、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a mixture of 28.6 g of 8-chloro-1,2,3,4-tetrahydoisoquinoline hydrochloride in 140 ml of dichloromethane was added 140 ml of 1N aqueous NaOH solution and 17.6 g of NaHCO3. To the solution was added dropwise 14.5 ml of acetic anhydride at 5° C. The mixture was stirred at room temperature for 1 hour. The organic layer was separated and the aqueous layer was extracted with dichloromethane. The combined organic extracts were washed with water, dried over anhydrous sodium sulfate. The solvent was distilled off to give 29.1 g of the title compound as a pale red oil.

後処理

  1. customThe organic layer was separated
  2. extractionthe aqueous layer was extracted with dichloromethane
  3. washThe combined organic extracts were washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-95ad5da48c2b4f3eac985c169b57df40
出典データセット
uspto-grants-1993_12
特許番号
US05273974

反応ノート

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