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Sodium Hydroxide → 5-Phenyl-[1,4]diazepane

HRID 1637166
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HRID 1637166 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

HCID 193479295-Phenyl-[1,4]diazepane수율 105.8%

시약·촉매·용매 2

HCID 962Water용매3회HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-667d7ebca57e4a919e0a31c6a303371c
출처 데이터셋
uspto-grants-2000_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06040303

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