1,1-Dichloroethane → HCID 118037735、化合物

HRID 587795

反応式

HRID 587795 の反応式
[N+:1]([C:4]([N+:8]([O-:10])=[O:9])(O)[CH2:5]C)([O-:3])=[O:2].[CH2:11]([CH:17]([CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:18]([OH:20])=[O:19])[CH2:12][CH2:13][CH2:14][CH2:15][CH3:16].Cl[CH:30](Cl)C>>[N+:1]([C:4]([N+:8]([O-:10])=[O:9])([CH3:5])[CH2:30][O:19][C:18](=[O:20])[CH:17]([CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])([O-:3])=[O:2]

参加物

4

反応物 3

HCID 63651,1-DichloroethaneHCID 329122-Hexyldecanoic acidHCID 54131844HCID 54131844、化合物

生成物 1

HCID 118037735HCID 118037735、化合物収率 60%

反応条件

温度
70 °C

実験手順

Dinitropropanol (25.5 g, 0.17 mol), 2-hexyldecanoic acid (48.7 g, 0.19 mol) and 50 g of polyphosphoric acid were added to 50 mL of dichloroethane and the resulting mixture was slowly stirred using a stirrer. The solution thus obtained was slowly heated to 70° C. and then reacted for 15 hr (overnight). After the reaction, the temperature of the reactor was lowered to room temperature, and the stirrer was powered off. When the temperature of the reactor was room temperature, the dichloroethane layer was decanted, followed by extraction with a 1 N sodium hydroxide aqueous solution and then distillation under reduced pressure, affording 2,2-dinitropropyl-2-hexyldecanoate (39.6 g, yield: 60%).

後処理

  1. customThe solution thus obtained
  2. customreacted for 15 hr (overnight)
  3. customAfter the reaction
  4. customwas lowered to room temperature
  5. customwas room temperature
  6. customthe dichloroethane layer was decanted
  7. extractionfollowed by extraction with a 1 N sodium hydroxide aqueous solution
  8. distillationdistillation under reduced pressure

出典と根拠

ORDレコード
ord-1ab3c6459ff0497190cbe0f2624b6bf0
出典データセット
uspto-grants-2016_01
特許番号
US09227910B2

関連ノート

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