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

HRID 1087970ノート

反応式

HRID 1087970 の反応式
[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]

参加物

3

反応物 2

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

生成物 1

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

反応条件

温度
130 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e08a171b5cee4274b723cba3e8ea35b9
出典データセット
uspto-grants-1990_10
特許番号
US04960924

反応ノート

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