2,2,5,5-Tetramethyl-3-hexanone → HCID 21135795、化合物

HRID 1042406ノート

反応式

HRID 1042406 の反応式
[CH3:1][C:2]([CH3:11])([C:4](=O)[CH2:5][C:6]([CH3:9])([CH3:8])[CH3:7])[CH3:3].[C:12](O)(=O)C.[CH:16]([NH2:18])=[NH:17]>C(O)CCC>[C:2]([C:4]1[C:5]([C:6]([CH3:9])([CH3:8])[CH3:7])=[CH:12][N:18]=[CH:16][N:17]=1)([CH3:11])([CH3:3])[CH3:1]

参加物

4

反応物 2

HCID 1366702,2,5,5-Tetramethyl-3-hexanoneHCID 160693Formamidine acetate

生成物 1

HCID 21135795HCID 21135795、化合物収率 43.3%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
130 °C

実験手順

A 100 mL reaction flask is charged with 2,2,5,5-tetramethyl-hexan-3-one (10 g, 0.06 mol), formamidine acetate (33 g, 0.3 mol), and butanol (50 mL). The reaction mixture is heated to 130° C. and stirred for 24 hours. The crude mass is washed once with aqueous sulfuric acid (10%, 100 mL) followed by twice with brine (30 mL). Butanol is recovered by roto-evaporation. The crude product is further purified with liquid chromatography (Biotage® system) and then crystallized. Product 4,5-di-tert-butyl-pyrimidine (˜5 g) is obtained.

後処理

  1. customA 100 mL reaction flask
  2. washThe crude mass is washed once with aqueous sulfuric acid (10%, 100 mL)
  3. customButanol is recovered by roto-evaporation
  4. customThe crude product is further purified with liquid chromatography (Biotage® system)
  5. customcrystallized

出典と根拠

ORDレコード
ord-d998b382f77b4e5fb204f88317e49027
出典データセット
uspto-grants-2013_10
特許番号
US08557876B2

反応ノート

読み込み中…