Formaldehyde → 3,7-Dimethyl-2-methylene-7-hydroxyoctanal

HRID 15623

반응식

HRID 15623 반응식
[CH3:1][CH:2]([CH2:10][CH:11]=[O:12])[CH2:3][CH2:4][CH2:5][C:6]([OH:9])([CH3:8])[CH3:7].C=O.[CH2:15](NCCCC)CCC.C(O)(=O)CCCCC>>[CH3:1][CH:2]([CH2:3][CH2:4][CH2:5][C:6]([CH3:8])([OH:9])[CH3:7])[C:10](=[CH2:15])[CH:11]=[O:12]

참가 물질

5

반응물 4

HCID 712FormaldehydeHCID 7888Hydroxycitronellal2회HCID 8148DibutylamineHCID 8892Hexanoic Acid

생성물 1

HCID 866322753,7-Dimethyl-2-methylene-7-hydroxyoctanal수율 1,341.5%

반응 조건

온도
95 °C

실험 절차

A 3 L four-necked flask equipped with a stirrer, a thermometer and a reflux condenser was charged with 1032 g (6.0 mol) of hydroxycitronellal, 520 g (6.4 mol) of a 37% by mass formaldehyde aqueous solution, 53 g (0.41 mol) of dibutyl amine and 10 g (0.09 mol) of hexanoic acid, and the contents in the flask were stirred while heating at 95° C. After the elapse of 40 min, it was confirmed that no hydroxycitronellal was present in the raw mixture, and then the mixture was cooled and separated into two layers. The thus separated organic layer was subjected to distillation treatment, thereby obtaining 1058 g (5.5 mol) of 3,7-dimethyl-2-methylene-7-hydroxyoctanal (purity as measured by gas chromatography: 95%) (yield based on theoretical amount: 92%).

후처리

  1. customA 3 L four-necked flask equipped with a stirrer
  2. customAfter the elapse of 40 min, it
  3. temperaturethe mixture was cooled
  4. customseparated into two layers
  5. distillationThe thus separated organic layer was subjected to distillation treatment

출처 및 근거

ORD 기록
ord-7f60cc2eaa174291a37a3a0e14fbbd2f
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732644B2

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