2,3-Butanediol → HCID 57720059, 화합물

HRID 1985590노트

반응식

HRID 1985590 반응식
[CH3:1][CH:2]([OH:6])[CH:3]([OH:5])[CH3:4].[C:7]1([CH3:17])[CH:12]=[CH:11][C:10](S(O)(=O)=O)=[CH:9][CH:8]=1.[C:18]1(C)C=CC=CC=1>>[CH3:4][CH:3]1[CH:2]([CH3:1])[O:6][C:8]2([CH:9]([CH3:18])[CH2:10][CH2:11][CH2:12][CH:7]2[CH3:17])[O:5]1

참가 물질

4

반응물 3

HCID 2622,3-ButanediolHCID 1140TolueneHCID 6101p-Toluenesulfonic acid

생성물 1

HCID 57720059HCID 57720059, 화합물

반응 조건

온도
120 °C

실험 절차

A reaction flask equipped with a Dean Stark trap was charged with 2,6-dimethyl cyclohehanone (200 g), 2,3-butanediol (315 g), p-toluenesulfonic acid (2 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 2,3,6,10-tetramethyl-1,4-dioxaspiro[4,5]decane (265 g)), which had a boiling point of 104° C. at a pressure of 16 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 the reaction mass
  5. temperaturewas cooled to an ambient temperature
  6. washwashed with brine
  7. customPurification
  8. distillationby vacuum distillation

출처 및 근거

ORD 기록
ord-23dfa52ab24445c69b979b71f0097541
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07547667B1

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