Methanol → HCID 178481705、化合物

HRID 444555

反応式

HRID 444555 の反応式
[C:1]([NH:5][NH2:6])(=O)[CH2:2][OH:3].[CH3:7][N:8]=[C:9]=[S:10].CO.[Na]>C(O)C>[OH:3][CH2:2][C:1]1[N:8]([CH3:7])[C:9]([SH:10])=[N:6][N:5]=1

参加物

6

反応物 4

HCID 887MethanolHCID 11167Methyl isothiocyanateHCID 3505362-HydroxyacetohydrazideHCID 5360545Sodium

生成物 1

HCID 178481705HCID 178481705、化合物収率 35.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 9 g of glycolic acid hydrazide, 7.3 g of methyl isothiocyanate, 50 ml of methanol and 50 ml of ethanol was heated under reflux for 5 hours. Following the addition of 2.3 g of sodium metal, the mixture was further refluxed for 24 hours. The reaction mixture was concentrated under reduced pressure and the residue was dissolved in 150 ml of water and adjusted to pH 2.5 with phosphoric acid. The resultant crystals were collected by filtration and recrystallized from ethanol. By the above procedure there were obtained 5.2 g of the captioned compound. m.p. 199°-201° C.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 5 hours
  3. temperaturethe mixture was further refluxed for 24 hours
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. dissolutionthe residue was dissolved in 150 ml of water
  6. filtrationThe resultant crystals were collected by filtration
  7. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-2a9cfc64dc5e44e7a2c3edc3180ea0a0
出典データセット
uspto-grants-1981_04
特許番号
US04264595

関連ノート

読み込み中…