Triethyl orthoacetate → HCID 14685529、化合物

HRID 1073115

反応式

HRID 1073115 の反応式
[N:1]12[CH2:8][CH2:7][CH:4]([CH2:5][CH2:6]1)[CH:3]([C:9]([NH:11][NH2:12])=[O:10])[CH2:2]2.[C:13](OCC)(OCC)(OCC)[CH3:14]>>[CH3:13][C:14]1[O:10][C:9]([CH:3]2[CH:4]3[CH2:7][CH2:8][N:1]([CH2:6][CH2:5]3)[CH2:2]2)=[N:11][N:12]=1

参加物

3

反応物 2

HCID 66221Triethyl orthoacetateHCID 573413Quinuclidine-3-carbohydrazide

生成物 1

HCID 14685529HCID 14685529、化合物収率 72%

反応条件

温度
140 °C

実験手順

(±) 1-Azabicyclo[2.2.2]octane-3-carboxylic acid hydrazide (D8) (0.36 g; 2.1 mmoles) and triethyl orthoacetate (3 ml) were heated at 120° C. for 2 h. Excess triethyl orthoacetate was evaporated in vacuo and the residue was heated for a further 2 h at 140° C. The reaction was diluted with water (10 ml), saturated with potassium carbonate and extracted into ether (3×15 ml). Combined organic extracts were dried (Na2SO4) and concentrated to give the title compound as an oil (0.29 g; 72%), which was purified as the oxalate salt. m.p. 147°-8° (Acetone-methanol).

後処理

  1. customExcess triethyl orthoacetate was evaporated in vacuo
  2. additionThe reaction was diluted with water (10 ml), saturated with potassium carbonate
  3. extractionextracted into ether (3×15 ml)
  4. dry with materialCombined organic extracts were dried (Na2SO4)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-dd78b628f6aa49dcb85345b4af5a8fbd
出典データセット
uspto-grants-1990_11
特許番号
US04968691

関連ノート

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