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Phosphorus oxide (P4O10) → p-Methyl-cinnaMoyl Azide

HRID 651587
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HRID 651587 반응식
[C:1]1([CH3:12])[CH:6]=[CH:5][C:4]([CH:7]=[CH:8][C:9](Cl)=[O:10])=[CH:3][CH:2]=1.[N-:13]=[N+:14]=[N-:15].[Na+].O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O>O1CCOCC1.O.O1CCOCC1>[C:1]1([CH3:12])[CH:6]=[CH:5][C:4]([CH:7]=[CH:8][C:9]([N:13]=[N+:14]=[N-:15])=[O:10])=[CH:3][CH:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 14812Phosphorus oxide (P4O10)HCID 33557Sodium AzideHCID 53411298p-Methylcinnamoyl chloride

생성물 1

HCID 53914129p-Methyl-cinnaMoyl Azide

시약·촉매·용매 2

HCID 312751,4-Dioxane용매HCID 218864351,4-Dioxane--water (1/1)용매

반응 조건

온도
7.5 °C

실험 절차

3-p-Tolyl-acryloyl chloride (22.3 g, 123.3 mmol) in dioxane (50 mL) is slowly added to an ice cooled solution of sodium azide (16 g, 246.6 mmol) in water/dioxane (50 mL, 1/1, v/v) so as to maintain the temperature between 5-10° C. The mixture is stirred for 1.5 hours then poured over 300 g of ice. The resulting white solid is filtered and washed with additional water. The solid (20.72 g, 110.7 mmol) was dried over P2O5 under vacuum overnight and used in the next step without further purification.

후처리

  1. filtrationThe resulting white solid is filtered
  2. washwashed with additional water
  3. customused in the next step without further purification

출처 및 근거

ORD 기록
ord-2cb7e8858e39471b9809495ab6419188
출처 데이터셋
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06281227B1

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