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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Phosphorus trichloride → HCID 20082255, 화합물

HRID 1609784
노트
인쇄 미리보기

반응식

HRID 1609784 반응식
[C:1]([C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=[C:7]([CH3:15])[C:6]=1[OH:16])([CH3:4])([CH3:3])[CH3:2].[P:17]([Cl:20])(Cl)Cl>CN(C)C=O.C1(C)C(C)=CC=CC=1>[C:1]([C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[CH:8]=[C:7]([CH3:15])[C:6]=1[O:16][P:17]([Cl:20])[O:16][C:6]1[C:7]([CH3:15])=[CH:8][C:9]([C:11]([CH3:13])([CH3:12])[CH3:14])=[CH:10][C:5]=1[C:1]([CH3:4])([CH3:3])[CH3:2])([CH3:4])([CH3:3])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 24387Phosphorus trichlorideHCID 692244,6-Di-tert-butyl-o-cresol

생성물 1

HCID 20082255HCID 20082255, 화합물수율 95%

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 7237O-Xylene용매

반응 조건

온도
50 °C

실험 절차

890.3 g (4 mol) of 2,4-di-tert-butyl-6-methylphenol, 4.2 g of dimethylformamide and 170.0 g of xylene are introduced into a four-neck flask which has been flushed with nitrogen and is fitted with a thermometer, dropping funnel, reflux condenser and distillation attachment. 274.9 g (2 mol) of phosphorus trichloride are added dropwise with stirring over the course of 1.5 hours at a temperature of 50° C. The reaction mixture is warmed to 130° C. and refluxed at this temperature for 1 hour. The reaction mixture is kept at 120° C. for 1 hour under a vacuum of 0.15 bar. Xylene is subsequently removed by distillation under a greater vacuum. After the vacuum has been broken using nitrogen, 959.5 g (1.9 mol) of the title compound are obtained as supercooled, yellow-orange, clear melt.

후처리

  1. customhas been flushed with nitrogen
  2. customis fitted with a thermometer
  3. temperaturereflux condenser
  4. distillationdistillation attachment
  5. temperatureThe reaction mixture is warmed to 130° C.
  6. temperaturerefluxed at this temperature for 1 hour
  7. waitThe reaction mixture is kept at 120° C. for 1 hour under a vacuum of 0.15 bar
  8. customXylene is subsequently removed by distillation under a greater vacuum

출처 및 근거

ORD 기록
ord-fe8bb390e62742689ba7acf0a2fca8fd
출처 데이터셋
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05401845

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