Methanol → HCID 86748585, compound

HRID 1609437Notes

Reaction equation

HRID 1609437 reaction equation
[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]

Participants

5

Reactant 3

HCID 887MethanolHCID 19051Acetic acid, 1-methylhydrazideHCID 86748586HCID 86748586, compound

Product 1

HCID 86748585HCID 86748585, compoundYield 66%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

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.

Workup

  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

Sources & evidence

ORD record
ord-7070d28be52e4242a964f3ecdc216272
Source dataset
uspto-grants-1995_03
Patent number
US05401621

Reaction notes

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