Benzyl formate → HCID 54271345, 화합물

HRID 476349

반응식

HRID 476349 반응식
[C:1]([OH:20])(=[O:19])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]([OH:18])=[O:17].C(O[CH2:24][C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)=O>CCCCCCCC>[CH2:24]([O:17][C:16](=[O:18])[CH2:15][CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][C:1]([OH:20])=[O:19])[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1

참가 물질

4

반응물 2

HCID 7708Benzyl formate2회HCID 10459Hexadecanedioic acid

생성물 1

HCID 54271345HCID 54271345, 화합물

시약·촉매·용매 1

HCID 356Octane용매

반응 조건

온도
20 °C

실험 절차

Hexadecanedioic acid (20.0 g, 69.8 mmol) and Dowex® were suspended in n-octane and heated to reflux. Benzyl formate (22.0 g, 162 mmol) was added. After 6 hours additional benzyl formate (22.0 g, 162 mmol) was added. The heating was continued for 50 hours. The reaction mixture was filtered at 80° C. The filtrate was cooled to 20° C., and the precipitate was collected by filtration. The crude product (20.2 g) was suspended in dichloromethane (220 ml) at 20° C. for 4 hours. The suspension was filtered, and the filtrate was evacuated to dryness at 20-30° C. The resulting solid (13.9 g) was recrystallised from 2-propanol (140 ml). The product was isolated by filtration, and dried to constant weight under reduced pressure at 30-40° C. Yield: 10.2 g (39%) of white material.

후처리

  1. temperatureheated to reflux
  2. filtrationThe reaction mixture was filtered at 80° C
  3. filtrationthe precipitate was collected by filtration
  4. waitThe crude product (20.2 g) was suspended in dichloromethane (220 ml) at 20° C. for 4 hours
  5. filtrationThe suspension was filtered
  6. customthe filtrate was evacuated to dryness at 20-30° C
  7. customThe resulting solid (13.9 g) was recrystallised from 2-propanol (140 ml)
  8. customThe product was isolated by filtration
  9. customdried to constant weight under reduced pressure at 30-40° C

출처 및 근거

ORD 기록
ord-5fac0035e8e44bb585875c74861c995b
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637647B2

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