Acetic Anhydride → HCID 12838038, 화합물

HRID 1447113노트

반응식

HRID 1447113 반응식
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.[C:13]([O-])(=[O:15])[CH3:14].[Na+].C(OC(=O)C)(=O)C>C(O)(=O)C>[C:13]([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:15])[CH3:14]

참가 물질

5

반응물 3

HCID 7918Acetic AnhydrideHCID 517045Sodium AcetateHCID 125950728-Chloro-1,2,3,4-tetrahydroisoquinoline hydrochloride

생성물 1

HCID 12838038HCID 12838038, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 20.4 g. (0.1 mole) 8-chloro-1,2,3,4-tetrahydroisoquinoline, hydrochloride, 9.85 g. (0.12 mole) sodium acetate 40 ml. acetic anhydride and 100 ml. acetic acid was heated for 3 hours on a steambath with stirring. After the solvent was removed under reduced pressure, the residue was dissolved in water which was then made basic with concentrated ammonium hydroxide. The crude product was extracted into methylene chloride and the organic solution was washed with water, 10% hydrochloric acid, water and 5% aqueous sodium bicarbonate. The organic solution was then dried over anhydrous magnesium sulfate and then concentrated to dryness under vacuum to afford 2-acetyl-8-chloro-1,2,3,4-tetrahydroisoquinoline as a yellow oil.

후처리

  1. additionA mixture of 20.4 g
  2. customAfter the solvent was removed under reduced pressure
  3. dissolutionthe residue was dissolved in water which
  4. extractionThe crude product was extracted into methylene chloride
  5. washthe organic solution was washed with water, 10% hydrochloric acid, water and 5% aqueous sodium bicarbonate
  6. dry with materialThe organic solution was then dried over anhydrous magnesium sulfate
  7. concentrationconcentrated to dryness under vacuum

출처 및 근거

ORD 기록
ord-f382f2d0f52648e1a116ec4774f6ae3b
출처 데이터셋
uspto-grants-1982_02
특허 번호
US04315935

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