Acetyl chloride → HCID 20392270, compound
Reaction equation
[CH:1]1[S:2][CH:3]=[C:4]2[C:10]=1[C:9](=[O:11])[NH:8][C:7]1[CH:12]=[CH:13][CH:14]=[CH:15][C:6]=1[NH:5]2.[C:16](Cl)(=[O:18])[CH3:17]>C1C=CC=CC=1>[C:16]([N:5]1[C:6]2[CH:15]=[CH:14][CH:13]=[CH:12][C:7]=2[NH:8][C:9](=[O:11])[C:10]2=[CH:1][S:2][CH:3]=[C:4]12)(=[O:18])[CH3:17]Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A reaction mixture comprising 9.9 g. of 4,9-dihydro-10H-thieno[3,4-b][1,5]benzodiazepin-10-one and 4 g. (3.7 ml.) of acetyl chloride in 100 ml. of benzene is refluxed for 3 hours and then allowed to stand at room temperature overnight. The precipitate is collected, washed with benzene and dried. The solid is crystallized twice from hot methanol with cooling giving the desired product, mp. 228°-230° C.
Workup
- customThe precipitate is collected
- washwashed with benzene
- customdried
- customThe solid is crystallized twice from hot methanol
- temperaturewith cooling
Sources & evidence
- ORD record
- ord-602f6f6541534e6ea0bf5aaff1b3e541
- Source dataset
- uspto-grants-1979_09
- Patent number
- US04168269
Reaction notes
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