Toluene → HCID 57720058, 화합물

HRID 1985593노트

반응식

HRID 1985593 반응식
[CH3:1][CH:2]([OH:7])[CH2:3][CH:4]([OH:6])[CH3:5].[C:8]1([CH3:18])[CH:13]=[CH:12][C:11](S(O)(=O)=O)=[CH:10][CH:9]=1.[C:19]1(C)C=CC=CC=1>>[CH3:5][CH:4]1[CH2:3][CH:2]([CH3:1])[O:7][C:9]2([CH:10]([CH3:19])[CH2:11][CH2:12][CH2:13][CH:8]2[CH3:18])[O:6]1

참가 물질

4

반응물 3

HCID 1140TolueneHCID 6101p-Toluenesulfonic acidHCID 122622,4-Pentanediol

생성물 1

HCID 57720058HCID 57720058, 화합물

반응 조건

온도
120 °C

실험 절차

A reaction flask equipped with a Dean Stark trap was charged with 2,6-dimethyl cyclohehanone (252 g), 2,4-pentanediol (312 g), p-toluenesulfonic acid (6 g) and toluene (300 mL). The reaction mass was heated to reflux (110-130° C.). Water (36 mL) was collected in the Dean Stark trap. When no water was recovered, the reaction mass was cooled to an ambient temperature, neutralized with 10% aqueous sodium carbonate (100 mL) and washed with brine. Purification by vacuum distillation afforded 2,4,7,11-tetramethyl-1,5-dioxaspiro[5,5]undecane (339 g), which had a boiling point of 124° C. at a pressure of 40 mmHg.

후처리

  1. customA reaction flask equipped with a Dean Stark trap
  2. temperatureThe reaction mass was heated
  3. customWater (36 mL) was collected in the Dean Stark trap
  4. customWhen no water was recovered
  5. temperaturethe reaction mass was cooled to an ambient temperature
  6. washwashed with brine
  7. customPurification
  8. distillationby vacuum distillation

출처 및 근거

ORD 기록
ord-fb988baafe3a43ea83de7719cdbf8854
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07547668B1

반응 노트

불러오는 중…