Ethyl chloroformate → HCID 21527848, compound
Reaction equation
[CH3:1][NH:2][NH:3][C:4]1[CH2:5][N:6]=[C:7]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[Cl:22])[C:8]2[CH:13]=[C:12]([CH2:14][CH3:15])[S:11][C:9]=2[N:10]=1.[C:23](Cl)(=[O:27])[O:24][CH2:25][CH3:26]>C(Cl)(Cl)Cl>[CH2:25]([O:24][C:23]([N:2]([CH3:1])[NH:3][C:4]1[CH2:5][N:6]=[C:7]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[Cl:22])[C:8]2[CH:13]=[C:12]([CH2:14][CH3:15])[S:11][C:9]=2[N:10]=1)=[O:27])[CH3:26]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
5 g of 2-(2-methylhydrazino)-5-o-chlorophenyl-7-ethyl-3H-thieno-[2,3-e][1,4]diazepine is dissolved in 30 ml of chloroform and a solution of 1.8 g of ethyl chlorocarbonate in 10 ml of chloroform is added dropwise with stirring, and the resulting mixture is stirred at room temperature for 2 hours. Then the reaction mixture is washed successively with water, an aqueous sodium hydrogen carbonate solution and water, and dried over anhydrous magnesium sulfate, and the chloroform is removed under reduced pressure. The residue is dissolved in ligroin, and the solution is allowed to stand overnight in a refrigerator to give 2-(2-ethoxycarbonyl-2-methylhydrazino)-5-o-chlorophenyl-7-ethyl-3H-thieno[2,3-e][1,4]diazepine appearing as pale yellow crystals, melting at 172°-174° C.
Workup
- stirringthe resulting mixture is stirred at room temperature for 2 hours
- washThen the reaction mixture is washed successively with water
- dry with materialan aqueous sodium hydrogen carbonate solution and water, and dried over anhydrous magnesium sulfate
- customthe chloroform is removed under reduced pressure
- dissolutionThe residue is dissolved in ligroin
Sources & evidence
- ORD record
- ord-892bb0a9e96548ce8598965667f44254
- Source dataset
- uspto-grants-1976_06
- Patent number
- US03965111
Reaction notes
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