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Sodium borohydride → 4-Acetylaminomethyl-1-ethyl-1,2,3,6-tetrahydropyridine

HRID 973995
ノート
印刷プレビュー

反応式

HRID 973995 の反応式
[BH4-].[Na+].[I-].[C:4]([NH:7][CH2:8][C:9]1[CH:14]=[CH:13][N+:12]([CH2:15][CH3:16])=[CH:11][CH:10]=1)(=[O:6])[CH3:5]>CO>[C:4]([NH:7][CH2:8][C:9]1[CH2:14][CH2:13][N:12]([CH2:15][CH3:16])[CH2:11][CH:10]=1)(=[O:6])[CH3:5]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 197755294-Acetylaminomethyl-1-ethylpyridinium iodide

生成物 1

HCID 150234574-Acetylaminomethyl-1-ethyl-1,2,3,6-tetrahydropyridine収率 88.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
75 °C

実験手順

Sodium borohydride (21.96 g) was added portionwise to a solution of 4-acetylaminomethyl-1-ethylpyridinium iodide (44.43 g) in methanol (400 ml) below 20° C. and the mixture was stirred at 75° C. for 3 hours. The mixture was evaporated in vacuo and the residue was poured into 0.7N aqueous solution of sodium hydroxide (115 ml). The mixture was extracted with methylene chloride. The extracts were washed with brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by vacuum distillation to give 4-acetylaminomethyl-1-ethyl-1,2,3,6-tetrahydropyridine (23.38 g).

後処理

  1. customThe mixture was evaporated in vacuo
  2. additionthe residue was poured into 0.7N aqueous solution of sodium hydroxide (115 ml)
  3. extractionThe mixture was extracted with methylene chloride
  4. washThe extracts were washed with brine
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo
  7. distillationThe residue was purified by vacuum distillation

出典と根拠

ORDレコード
ord-7cedd8e75b1b44009c1c9af09a299115
出典データセット
uspto-grants-1991_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05066680

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート