Hydrazine → 1-(2-Hydroxyethyl)-2-hydrazinoimidazoline mesylate

HRID 256542

反応式

HRID 256542 の反応式
[S:1]([OH:5])(=[O:4])(=[O:3])[CH3:2].[OH:6][CH2:7][CH2:8][N:9]1[CH2:13][CH2:12][N:11]=[C:10]1SC.[NH2:16][NH2:17]>C(O)C.COC(C)(C)C>[S:1]([OH:5])(=[O:4])(=[O:3])[CH3:2].[OH:6][CH2:7][CH2:8][N:9]1[CH2:13][CH2:12][N:11]=[C:10]1[NH:16][NH2:17]

参加物

5

反応物 2

HCID 9321HydrazineHCID 197853791-(2-Hydroxyethyl)-2-methylthioimidazoline mesylate

生成物 1

HCID 197854081-(2-Hydroxyethyl)-2-hydrazinoimidazoline mesylate

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 15413tert-Butyl methyl ether溶媒

実験手順

1-(2-Hydroxyethyl)-2-methylthioimidazoline mesylate (35 g, 0.136 mole) is suspended in ethyl alcohol (80 ml) and treated with anhydrous hydrazine (9.3 ml, 0.296 mole). The mixture became clear immediately. The solution is stirred at room temperature overnight and then diluted with t-butyl methyl ether (1 liter). On storage of the mixture in the freezer at -20° C., crystals separated, which are filtered, washed well with t-butyl methyl ether and dried. Recrystallization from isopropyl alcohol and t-butyl methyl ether gives 1-(2-hydroxyethyl)-2-hydrazinoimidazoline mesylate, melting point 85°-88° C.

後処理

  1. customOn storage of the mixture in the freezer at -20° C., crystals separated
  2. filtrationwhich are filtered
  3. washwashed well with t-butyl methyl ether
  4. customdried
  5. customRecrystallization from isopropyl alcohol and t-butyl methyl ether

出典と根拠

ORDレコード
ord-c9809d95a10348d3ab8f28f924a495e8
出典データセット
uspto-grants-1993_11
特許番号
US05258381

関連ノート

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