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

HRID 256542

반응식

HRID 256542 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매HCID 15413tert-Butyl methyl ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c9809d95a10348d3ab8f28f924a495e8
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05258381

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