Hydrogen Sulfide → HCID 54565844、化合物

HRID 1076048ノート

反応式

HRID 1076048 の反応式
[Na].[CH2:2]([O:4][C:5](=[O:13])[CH:6]=[CH:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[CH3:3].[SH2:14]>C(O)C>[CH2:2]([O:4][C:5](=[O:13])[CH2:6][CH:7]([SH:14])[CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[CH3:3]

参加物

5

反応物 3

HCID 402Hydrogen Sulfide2 回HCID 238322-Octenoic acid ethyl esterHCID 5360545Sodium

生成物 1

HCID 54565844HCID 54565844、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

0.2 g of sodium are dissolved in 10 ml of absolute ethyl alcohol. After completed alcoholate-formation, 5 g of 2-octenoic acid ethyl ester are added and the solution is cooled to -70°. At this temperature, 10 ml of hydrogen sulphide are condensed into the solution. Subsequently, the whole mixture is immediately transferred into an autoclave, pre-cooled to about -30°, and left by itself overnight at room temperature in the sealed pressure vessel. On the next morning, the autoclave is heated at 50° for a further 2 hours. After cooling to room temperature, the excess hydrogen sulphide is vented off, the reaction product washed with saturated common salt solution, dried and distilled. There are obtained 1.6 g of 3-mercapto-octanoic acid ethyl ester of boiling point 74°/0.4 mm Hg, nD20 1.4538.

後処理

  1. additionare added
  2. temperaturethe solution is cooled to -70°
  3. customcondensed into the solution
  4. temperaturepre-cooled to about -30°
  5. temperatureOn the next morning, the autoclave is heated at 50° for a further 2 hours
  6. washthe reaction product washed with saturated common salt solution
  7. customdried
  8. distillationdistilled

出典と根拠

ORDレコード
ord-4127d53e387548a3afeb44448a25c778
出典データセット
uspto-grants-1976_05
特許番号
US03954843

反応ノート

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