Triethylamine → HCID 178454912, 화합물

HRID 1654466노트

반응식

HRID 1654466 반응식
[CH2:1]([PH:5](=[O:7])[OH:6])[CH2:2][CH2:3][CH3:4].[CH2:8](N(CC)CC)[CH3:9].C(OC(Cl)=O)C>ClCCl>[CH2:8]([O:7][PH:5]([CH2:1][CH2:2][CH2:3][CH3:4])=[O:6])[CH3:9]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 178454911HCID 178454911, 화합물

생성물 1

HCID 178454912HCID 178454912, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

51 g of n-butyphosphinic acid are dissolved in 200 ml of dichloromethane, the solution is cooled to 10°, and 42.3 g of triethylamine are added dropwise. An exothermic reaction takes place. The mixture is cooled to 10° again and 45.3 g of chloroformic acid ethyl ester are added dropwise within a period of 75 minutes. A precipitate forms in an exothermic reaction with the evolution of gas. A further 200 ml of dichloromethane are then added and the mixture is allowed to warm to room temperature and is then stirred for 2 hours at room temperature, washed with water and dried over sodium sulfate, and the organic solvent is removed. The crude product is distilled under a high vacuum, yielding n-butylphosphinic acid ethyl ester having a boiling point of 95° (5×10-5 bar).

후처리

  1. temperaturethe solution is cooled to 10°
  2. customAn exothermic reaction
  3. temperatureThe mixture is cooled to 10° again
  4. customA precipitate forms in an exothermic reaction with the evolution of gas
  5. washwashed with water
  6. dry with materialdried over sodium sulfate
  7. customthe organic solvent is removed
  8. distillationThe crude product is distilled under a high vacuum

출처 및 근거

ORD 기록
ord-e385a2e81ff14920ae9de186c908e0bc
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05407922

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