Acetyl chloride → HCID 20392270, compound

HRID 1863164Notes

Reaction equation

HRID 1863164 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

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

  1. customThe precipitate is collected
  2. washwashed with benzene
  3. customdried
  4. customThe solid is crystallized twice from hot methanol
  5. temperaturewith cooling

Sources & evidence

ORD record
ord-602f6f6541534e6ea0bf5aaff1b3e541
Source dataset
uspto-grants-1979_09
Patent number
US04168269

Reaction notes

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