1,1-Dichloroethane → HCID 118037735, 화합물

HRID 587795

반응식

HRID 587795 반응식
[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]

참가 물질

4

반응물 3

HCID 63651,1-DichloroethaneHCID 329122-Hexyldecanoic acidHCID 54131844HCID 54131844, 화합물

생성물 1

HCID 118037735HCID 118037735, 화합물수율 60%

반응 조건

온도
70 °C

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-1ab3c6459ff0497190cbe0f2624b6bf0
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09227910B2

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