Acetic Acid → HCID 22016025, 화합물

HRID 1451989노트

반응식

HRID 1451989 반응식
[OH2:1].C[CH:3]([CH2:7][CH2:8][CH2:9][CH:10]([CH3:15])[CH2:11][CH2:12][CH:13]=[O:14])[CH2:4]C=O.[C:16]([OH:19])(=[O:18])[CH3:17]>>[CH3:4][CH:3]([CH2:7][CH2:8][CH2:9][CH:10]([CH3:15])[CH2:11][CH2:12][C:13]([OH:1])=[O:14])[CH2:17][C:16]([OH:19])=[O:18]

참가 물질

4

반응물 3

HCID 176Acetic Acid2회HCID 962WaterHCID 19973343HCID 19973343, 화합물

생성물 1

HCID 22016025HCID 22016025, 화합물수율 61%

반응 조건

온도
50 °C

실험 절차

A 5-L pressure reaction vessel was charged with 0.19 g of Cu(OCOCH3)2 (H2O) and 1.5 L of acetic acid, and the vessel was pressurized to 7 atm with air and then warmed to 50° C. While air was introduced at a rate of 240 L/hr, a mixture of 750 g of 3,7-dimethyldecanedial and 750 mL of acetic acid was fed thereto over a period of 3 hours. After completion of the feed, the reaction was conducted for an additional 6 hours at the same temperature and pressure. The reaction vessel was cooled, the gas therein was purged and then the reaction mixture was taken out. This mixture was heated at 110° C. for 1 hour under nitrogen atmosphere. The acetic acid was distilled off under a reduced pressure and the residual liquid was distilled to give 3,7-dimethyldecanedioic acid as an almost colorless clear liquid having a boiling point of 175° to 180° C. at 0.80 mmHg. The yield was 61% (435 g). Instrumental-analysis data are shown below.

후처리

  1. additionWhile air was introduced at a rate of 240 L/hr
  2. waitAfter completion of the feed, the reaction was conducted for an additional 6 hours at the same temperature and pressure
  3. temperatureThe reaction vessel was cooled
  4. customthe gas therein was purged
  5. temperatureThis mixture was heated at 110° C. for 1 hour under nitrogen atmosphere
  6. distillationThe acetic acid was distilled off under a reduced pressure
  7. distillationthe residual liquid was distilled

출처 및 근거

ORD 기록
ord-f6f3e09be30c496896f3a8714d63aa42
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05606005

반응 노트

불러오는 중…