2-Mercaptoethanol → Butanoic acid, 3-oxo-, 2-mercaptoethyl ester

HRID 1087970노트

반응식

HRID 1087970 반응식
[SH:1][CH2:2][CH2:3][OH:4].[CH3:5][C:6]1[O:12]C(C)(C)O[C:8](=[O:9])[CH:7]=1>>[SH:1][CH2:2][CH2:3][O:4][C:8](=[O:9])[CH2:7][C:6]([CH3:5])=[O:12]

참가 물질

3

반응물 2

HCID 15672-MercaptoethanolHCID 793682,2,6-Trimethyl-4H-1,3-dioxin-4-one

생성물 1

HCID 10844726Butanoic acid, 3-oxo-, 2-mercaptoethyl ester수율 90%

반응 조건

온도
130 °C

실험 절차

In a 300 ml. round bottom flask fitted with a thermometer, mechanical stirrer, Dean Stark trap and reflux condenser was placed 25.0g.(0.32 mole) of 2-mercaptoethanol. This was stirred and heated to 130° C.; 45.4g. (0.32 mole) of 2,2,6-trimethyl-1,3-dioxen-4-one (TKD) was added dropwise at a uniform rate over the period of one hour. Heating was continued for 1/2 hour; acetone distillate was collected in the Dean Stark trap. After distillate collection was completed, the mixture was distilled under vacuum and the portion boiling at 110°-115° C.(at 5 mm. Hg.) was collected to give a colorless liquid of mercaptoethylacetoacetate. The yield was about 90% based on starting material. The product was identified by NMR spectroscopy.

후처리

  1. customround bottom flask fitted with a thermometer, mechanical stirrer, Dean Stark trap
  2. temperaturereflux condenser
  3. temperatureHeating
  4. distillationacetone distillate was collected in the Dean Stark trap
  5. distillationAfter distillate collection
  6. distillationthe mixture was distilled under vacuum
  7. customthe portion boiling at 110°-115° C.(at 5 mm. Hg.) was collected

출처 및 근거

ORD 기록
ord-e08a171b5cee4274b723cba3e8ea35b9
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04960924

반응 노트

불러오는 중…