Acetic Anhydride → HCID 12838038、化合物

HRID 1447113ノート

反応式

HRID 1447113 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.[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]

参加物

5

反応物 3

HCID 7918Acetic AnhydrideHCID 517045Sodium AcetateHCID 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 176Acetic Acid溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f382f2d0f52648e1a116ec4774f6ae3b
出典データセット
uspto-grants-1982_02
特許番号
US04315935

反応ノート

読み込み中…