Sulfuric Acid → Butyl tert-butoxyacetate

HRID 4370

反応式

HRID 4370 の反応式
[CH3:1][C:2](=[CH2:4])[CH3:3].[C:5]([O:9][CH2:10][CH2:11][CH2:12][CH3:13])(=[O:8])[CH2:6][OH:7].S(=O)(=O)(O)O>C(Cl)Cl>[C:2]([O:7][CH2:6][C:5]([O:9][CH2:10][CH2:11][CH2:12][CH3:13])=[O:8])([CH3:3])([CH3:1])[CH3:4]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 8255IsobutyleneHCID 81882Butyl Glycolate

生成物 1

HCID 14050415Butyl tert-butoxyacetate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A 500-ml, thick-walled Erlenynmeyer flask equipped with a magnetic stirring bar was cooled to -78° C. (dry iece-acetone bath) and charged with isobutylene (150 ml). Then, n-butyl glycolate (20.0 g, 0.151 mol) and 50 ml of methylene chloride was added along with 1 ml of concentrated sulfuric acid. The cold bath was removed and the mixture stirred for 3 days at room temperature. The reaction was quenched with 50 ml of saturated sodium bicarbonate and the product extracted with ether. The ether layer was dried over sodium sulfate and concentrated. After distillation, the title compound was obtained as a colorless oil: bp 64°-65° C. (0.7 mm).

後処理

  1. customA 500-ml, thick-walled Erlenynmeyer flask equipped with a magnetic stirring bar
  2. customThe cold bath was removed
  3. customThe reaction was quenched with 50 ml of saturated sodium bicarbonate
  4. extractionthe product extracted with ether
  5. dry with materialThe ether layer was dried over sodium sulfate
  6. concentrationconcentrated
  7. distillationAfter distillation

出典と根拠

ORDレコード
ord-97da413a676c4eefa7c6d0c7176edaf1
出典データセット
uspto-grants-1988_02
特許番号
US04725620

関連ノート

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