Methanol → Sodium 1-acetyl-1-methyl-4-sulfoethylthiosemicarbazide

HRID 1609437ノート

反応式

HRID 1609437 の反応式
[S:1]([CH2:5][CH2:6][N:7]=[C:8]=[S:9])([OH:4])(=[O:3])=[O:2].[Na:10].CO.[C:13]([N:16]([CH3:18])[NH2:17])(=[O:15])[CH3:14]>O>[C:13]([N:16]([CH3:18])[NH:17][C:8]([NH:7][CH2:6][CH2:5][S:1]([OH:4])(=[O:3])=[O:2])=[S:9])(=[O:15])[CH3:14].[Na:10]

参加物

5

反応物 3

HCID 887MethanolHCID 19051Acetic acid, 1-methylhydrazideHCID 86748586Sodium sulfoethylisothiocyanate

生成物 1

HCID 86748585Sodium 1-acetyl-1-methyl-4-sulfoethylthiosemicarbazide収率 66%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

175.3 g of sodium sulfoethylisothiocyanate was added to a solution obtained by adding 600 ml of methyl alcohol and 300 ml of water to 114.2 g of 1-acetyl-1-methylhydrazine. The system was then heated under reflux for 4 hours. After the reaction, the reaction solution was dried under reduced pressure. The resulting solid matter was then recrystallized from 1 l of methyl alcohol to obtain 169.4 g (yield: 66.0%) of the desired compound. m.p. 255°-256° C.

後処理

  1. customobtained
  2. temperatureThe system was then heated
  3. temperatureunder reflux for 4 hours
  4. customAfter the reaction
  5. customthe reaction solution was dried under reduced pressure
  6. customThe resulting solid matter was then recrystallized from 1 l of methyl alcohol

出典と根拠

ORDレコード
ord-7070d28be52e4242a964f3ecdc216272
出典データセット
uspto-grants-1995_03
特許番号
US05401621

反応ノート

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