Acetic Anhydride → HCID 18458647、化合物

HRID 1976275ノート

反応式

HRID 1976275 の反応式
[OH:1][CH:2]1[C:7]([C:8]2[C:13]([O:14][CH3:15])=[CH:12][C:11]([O:16][CH3:17])=[CH:10][C:9]=2[O:18][CH3:19])=[CH:6][CH2:5][N:4]([CH3:20])[CH2:3]1.[C:21](OC(=O)C)(=[O:23])[CH3:22]>>[C:21]([O:1][CH:2]1[C:7]([C:8]2[C:13]([O:14][CH3:15])=[CH:12][C:11]([O:16][CH3:17])=[CH:10][C:9]=2[O:18][CH3:19])=[CH:6][CH2:5][N:4]([CH3:20])[CH2:3]1)(=[O:23])[CH3:22]

参加物

3

反応物 2

HCID 7918Acetic AnhydrideHCID 99256571,2,3,6-Tetrahydro-1-methyl-4-(2,4,6-trimethoxyphenyl)-3-pyridinol

生成物 1

HCID 18458647HCID 18458647、化合物

反応条件

温度
100 °C

実験手順

2.79 g (10 mmol) of 3(R,S)-hydroxy-1-methyl4-(2,4,6-trimethoxyphenyl)-1,2,3,6-tetrahydropyridine (VII) were dissolved in 15 ml of acetic anhydride and stirred at 100° C. for 4 h. The solution was then evaporated in vacuo in a rotary evaporator and the residue was dissolved in 10 ml of water, adjusted to pH >12 with sodium hydroxide solution and extracted twice with 20 ml of ethyl acetate each time. The combined organic phases were washed with 10 ml of saturated sodium chloride solution, then dried over sodium sulfate and evaporated in vacuo on a rotary evaporator.

後処理

  1. customThe solution was then evaporated in vacuo in a rotary evaporator
  2. dissolutionthe residue was dissolved in 10 ml of water
  3. extractionextracted twice with 20 ml of ethyl acetate each time
  4. washThe combined organic phases were washed with 10 ml of saturated sodium chloride solution
  5. dry with materialdried over sodium sulfate
  6. customevaporated in vacuo on a rotary evaporator

出典と根拠

ORDレコード
ord-1bde4dd9709d43afbd9084578a2f6654
出典データセット
uspto-grants-2001_05
特許番号
US06225473B1

反応ノート

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