Acetic Acid → HCID 22016025、化合物

HRID 1451989ノート

反応式

HRID 1451989 の反応式
[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]

参加物

4

反応物 3

HCID 176Acetic Acid2 回HCID 962WaterHCID 19973343HCID 19973343、化合物

生成物 1

HCID 22016025HCID 22016025、化合物収率 61%

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f6f3e09be30c496896f3a8714d63aa42
出典データセット
uspto-grants-1997_02
特許番号
US05606005

反応ノート

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