Acetic Acid → 1,3-Bis(1-methylethoxy)-2-propanol

HRID 1050889

반응식

HRID 1050889 반응식
[CH:1]([O:4][CH2:5][CH:6]1[CH2:8][O:7]1)([CH3:3])[CH3:2].[CH3:9][CH:10]([CH3:12])[O-:11].[K+].C(O)(=O)C>CCCCCC.C(O)(C)C>[CH:10]([O:11][CH2:8][CH:6]([OH:7])[CH2:5][O:4][CH:1]([CH3:3])[CH3:2])([CH3:12])[CH3:9]

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 199202-((1-Methylethoxy)methyl)oxiraneHCID 23663646Potassium propan-2-olate

생성물 1

HCID 830521,3-Bis(1-methylethoxy)-2-propanol

시약·촉매·용매 2

HCID 3776Isopropanol용매2회HCID 8058Hexane용매

반응 조건

온도
80 °C

실험 절차

2-(Isopropoxymethyl)oxirane (23.23 g, 25.1 mL, 200 mmol) was dissolved in hexane (20 mL) and placed in reactor. Separately (1.2 g, 20 mmol) of KH was slowly added to (90.1 g, 115 mL, 1.5 Mol) of isopropanol at RT. After deprotonation was complete the solution of potassium isopropoxide in isopropanol was added to the reactor. All operations were performed in a glove box. The reactor was sealed and heated 80° C. for 24 hours. After cooling acetic acid (20 mmols) and ca. 5 g. of powdered talc were added to the reaction mixture followed by filtration through a plug of celite. The solvent was evaporated and the residue distilled under vacuum affording 20.09 g of 1,3-diisopropoxypropan-2-ol.

후처리

  1. customplaced in reactor
  2. additionwas added to the reactor
  3. customAll operations were performed in a glove box
  4. customThe reactor was sealed
  5. filtrationfollowed by filtration through a plug of celite
  6. customThe solvent was evaporated
  7. distillationthe residue distilled under vacuum

출처 및 근거

ORD 기록
ord-058682eadab8481ea18e4183af0407f7
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09388106B2

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