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

HRID 1050889

反応式

HRID 1050889 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3776Isopropanol溶媒2 回HCID 8058Hexane溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-058682eadab8481ea18e4183af0407f7
出典データセット
uspto-grants-2016_07
特許番号
US09388106B2

関連ノート

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