Sodium borohydride → HCID 10632014, compound

HRID 654064Notes

Reaction equation

HRID 654064 reaction equation
[BH4-].[Na+].N1([CH:9]2[NH:15][C:14](=[O:16])[C:13]3[S:17][CH:18]=[CH:19][C:12]=3[N:11]3[CH:20]=[CH:21][CH:22]=[C:10]23)CCCCC1>CO>[O:16]=[C:14]1[C:13]2[S:17][CH:18]=[CH:19][C:12]=2[N:11]2[CH:20]=[CH:21][CH:22]=[C:10]2[CH2:9][NH:15]1

Participants

4

Reactant 2

HCID 4311764Sodium borohydrideHCID 10850843HCID 10850843, compound

Product 1

HCID 10632014HCID 10632014, compoundYield 84%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

1 g (0.0028 mol) of sodium borohydride is added in small portions to a solution of 2 g (0.007 mol) of 6-piperidino-5,6-dihydro-4-oxo-4H-pyrrolo[1,2-a]thieno -[2,3-f][1,4]diazepine in 120 ml of methanol, and the reaction mixture is stirred at room temperature for 15 minutes and then heated to reflux for 30 minutes. The methanol is then removed under vacuum and the solid residue ground in 200 ml of water. The precipitate is drained, washed with water, dried and recrystallized. 1.2 g of 5,6-dihydro-4-oxo-4H-pyrrolo[1,2-a]-thieno[2,3-f][1,4]diazepine are obtained in the form of white crystals, melting point 191° C. (ethyl ether).

Workup

  1. temperatureheated
  2. temperatureto reflux for 30 minutes
  3. customThe methanol is then removed under vacuum
  4. washwashed with water
  5. customdried
  6. customrecrystallized

Sources & evidence

ORD record
ord-154e5f38feab4a70918056aafaab89d6
Source dataset
uspto-grants-1992_07
Patent number
US05130301

Reaction notes

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