Ammonia → HCID 12522172, compound

HRID 1658933Notes

Reaction equation

HRID 1658933 reaction equation
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[CH:9]([C:13]([O:15]C)=O)[N:8]=[C:7]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[C:6]=2[CH:23]=1.[NH3:24]>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[CH:9]([C:13](=[O:15])[NH2:24])[N:8]=[C:7]([C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)[C:6]=2[CH:23]=1

Participants

4

Reactant 2

HCID 222AmmoniaHCID 11198258HCID 11198258, compound

Product 1

HCID 12522172HCID 12522172, compoundYield 74%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

10 g. of 7-chloro-3-methoxycarbonyl-5-phenyl-2-oxo-2,3-dihydro-1H-benzo[f]-1,4-diazepine and 200 ml. of a 13.6% solution of ammonia in methanol are left together overnight at room temperature. The solid rapidly dissolves and after several hours a precipitate gradually forms which increases in quantity with passage of time, until the whole mass has solidified. The solid is filtered by suction and washed with methanol. An additional small quantity of the same product is obtained by concentrating the solution to dryness. The two crops are combined and recrystallized from methanol. Colorless crystals are obtained (7 g.); m.p. 255°-256°C.; yield 74%.

Workup

  1. dissolutionThe solid rapidly dissolves and after several hours a precipitate
  2. temperatureincreases in quantity with passage of time, until the whole mass
  3. filtrationThe solid is filtered by suction
  4. washwashed with methanol
  5. customAn additional small quantity of the same product is obtained
  6. concentrationby concentrating the solution to dryness
  7. customrecrystallized from methanol
  8. customColorless crystals are obtained (7 g.)

Sources & evidence

ORD record
ord-12eee3607f7f4b2cb86b2bcfd2152fd4
Source dataset
uspto-grants-1976_06
Patent number
US03966793

Reaction notes

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