Water → HCID 12519156, compound

HRID 2052710Notes

Reaction equation

HRID 2052710 reaction equation
Cl.[Cl:2][C:3]1[CH:4]=[C:5]2[C:9]3=[C:10]([CH:20]=1)[C:11]([CH3:19])=[N:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[N:8]3[CH2:7][CH2:6]2.[BH4-].[Na+].O>C(O)C>[Cl:2][C:3]1[CH:4]=[C:5]2[C:9]3=[C:10]([CH:20]=1)[CH:11]([CH3:19])[NH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[N:8]3[CH2:7][CH2:6]2

Participants

5

Reactant 3

HCID 962WaterHCID 4311764Sodium borohydrideHCID 12519144HCID 12519144, compound

Product 1

HCID 12519156HCID 12519156, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

To a well stirred mixture of 45.0 g of 4-chloro-6-methyl-1,2-dihydroindolo[1,7-ab][1,5]benzodiazepine hydrochloride, in 450 ml of absolute ethanol, cooled to 0° C. under N2, is added sodium borohydride in portions until the initial purple color is discharged. The mixture is stirred 1 hour longer at 0° C., then 2 hours at room temperature. Then water is added in portions to destroy excess reagent and to maximize precipitation of product. The latter is filtered, washed well with water and dried to yield 4-chloro-6-methyl-1,2,6,7-tetrahydroindolo[1,7-ab][1,5]benzodiazepine, m.p. 167°-170° C.

Workup

  1. stirringThe mixture is stirred 1 hour longer at 0° C.
  2. custom2 hours
  3. customat room temperature
  4. customto destroy excess reagent
  5. customprecipitation of product
  6. filtrationThe latter is filtered
  7. washwashed well with water
  8. customdried

Sources & evidence

ORD record
ord-09b3c994527c4845a827676807411805
Source dataset
uspto-grants-1980_01
Patent number
US04186199

Reaction notes

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