Acetyl chloride → HCID 21546072, compound

HRID 1606182Notes

Reaction equation

HRID 1606182 reaction equation
[C:1](Cl)(=[O:3])[CH3:2].[CH:5]1([N:8]2[C:17]3[CH2:16][CH2:15][CH2:14][NH:13][CH2:12][C:11]=3[CH:10]=[C:9]2[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH2:7][CH2:6]1.C(N(CC)CC)C>C(Cl)(Cl)Cl>[CH:5]1([N:8]2[C:17]3[CH2:16][CH2:15][CH2:14][N:13]([C:1](=[O:3])[CH3:2])[CH2:12][C:11]=3[CH:10]=[C:9]2[C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH2:6][CH2:7]1

Participants

5

Reactant 3

HCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 21546093HCID 21546093, compound

Product 1

HCID 21546072HCID 21546072, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent2×

Procedure

A solution of 3.9 g. of acetyl chloride in 25 ml. of chloroform is added to a cooled solution of 11.0 g. of 1-cyclopropyl-2-phenyl-1,4,5,6,7,8-hexahydropyrrolo[3,2-c]azepine and 5.0 g. of triethylamine in 50 ml. of dry chloroform. The mixture is stirred at ambient temperature for 20 hours, washed with water, dried, and concentrated to provide 1-cyclopropyl-2-phenyl-5-acetyl-1,4,5,6,7,8-hexahydropyrrolo[3,2-c]azepine as an oil. The oil is treated according to the manipulative procedure described above in Example 2, to give crystals, m.p. 85°C. dec., of 1-cyclopropyl-2-phenyl-5-ethyl-1,4,5,6,7,8-hexahydropyrrolo[3,2-c]azepine oxalate.

Workup

  1. washwashed with water
  2. customdried
  3. concentrationconcentrated

Sources & evidence

ORD record
ord-d125d67e0fa14ca0aa1326a7c2f29173
Source dataset
uspto-grants-1976_04
Patent number
US03952025

Reaction notes

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