Sodium borohydride → HCID 178505865, compound

HRID 1840632Notes

Reaction equation

HRID 1840632 reaction equation
[BH4-].[Na+].[Cl:3][C:4]1[CH:5]=[C:6]([NH:11][C:12]2[C:13]3[N:22]=[C:21]([Cl:23])[N:20]=[C:19](Cl)[C:14]=3[N:15]=[C:16]([Cl:18])[N:17]=2)[CH:7]=[CH:8][C:9]=1[F:10]>O.[OH-].[Na+].C(OCC)(=O)C>[Cl:3][C:4]1[CH:5]=[C:6]([NH:11][C:12]2[C:13]3[N:22]=[C:21]([Cl:23])[NH:20][CH2:19][C:14]=3[N:15]=[C:16]([Cl:18])[N:17]=2)[CH:7]=[CH:8][C:9]=1[F:10]

Participants

6

Reactant 2

HCID 4311764Sodium borohydrideHCID 12972393HCID 12972393, compound

Product 1

HCID 178505865HCID 178505865, compound

Reagents, catalysts & solvents 3

HCID 962WaterSolventHCID 8857Ethyl AcetateSolventHCID 14798Sodium HydroxideSolvent

Conditions

Temperature
10 °C

Procedure

At 2° C. a solution of 191.99 g (5.079 mol) of sodium borohydride in 520 ml of water and 22 ml of 2N sodium hydroxide solution is added dropwise to a suspension of 1100 g (2.902 mol) of (1) in 22 l of ethyl acetate. The mixture is stirred for 2 hours at 10° C. and then heated to 71° C. The suspension is filtered through Celite and cooled to 0° C. The product that crystallises out is filtered off and dried at 40° C. until a constant weight is attained.

Workup

  1. temperatureheated to 71° C
  2. filtrationThe suspension is filtered through Celite
  3. temperaturecooled to 0° C
  4. customThe product that crystallises out
  5. filtrationis filtered off
  6. customdried at 40° C. until a constant weight

Sources & evidence

ORD record
ord-71ba7e314c474ebab86d695e876610b6
Source dataset
uspto-grants-2004_01
Patent number
US06680384B2

Reaction notes

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