Sodium Hydroxide → HCID 19347929, compound

HRID 1637166Notes

Reaction equation

HRID 1637166 reaction equation
[H-].[H-].[H-].[H-].[Li+].[Al+3].[C:7]1([CH:13]2[NH:19][CH2:18][CH2:17][NH:16][C:15](=O)[CH2:14]2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[OH-].[Na+]>C1COCC1.O>[C:7]1([CH:13]2[NH:19][CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

Participants

6

Reactant 3

HCID 14798Sodium HydroxideHCID 130482357-Phenyl-1,4-diazepan-5-oneHCID 21226445Aluminium lithium hydride

Product 1

HCID 19347929HCID 19347929, compoundYield 105.8%

Reagents, catalysts & solvents 2

HCID 962WaterSolvent3×HCID 8028TetrahydrofuranSolvent

Procedure

2.0 g LiAlH4 were suspended in THF under a nitrogen atmosphere, and then 5.0 g hexahydro-7-phenyl-1,4-diazepin-5-one were added thereto at 10° C. Then the mixture was stirred for 8 hours at room temperature. Under a nitrogen atmosphere, 5 ml water, 2.2 g NaOH, dissolved in 5 ml water, and again 3 ml water were then added dropwise in succession, and the mixture was stirred for 15 minutes at room temperature. Once the resulting salts had been filtered out, the filtrate was reduced to dryness under vacuum. 4.9 g of 7-phenyl-1,4-diazepane were obtained, which was reacted without further purification.

Workup

  1. customat 10° C
  2. stirringthe mixture was stirred for 15 minutes at room temperature
  3. filtrationOnce the resulting salts had been filtered out

Sources & evidence

ORD record
ord-667d7ebca57e4a919e0a31c6a303371c
Source dataset
uspto-grants-2000_03
Patent number
US06040303

Reaction notes

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