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Phosphorus oxychloride → HCID 71743137, 화합물

HRID 633614
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HRID 633614 반응식
O[C:2]1[C:7]([NH:8][C:9](=[O:20])[C:10]2[CH:15]=[C:14]([CH3:16])[C:13]([O:17][CH3:18])=[C:12]([CH3:19])[CH:11]=2)=[C:6](O)[N:5]=[C:4]([S:22][CH3:23])[N:3]=1.S(=O)(=O)(O)[O-].[Na+].P(Cl)(Cl)([Cl:32])=O>>[Cl:32][C:2]1[C:7]2[N:8]=[C:9]([C:10]3[CH:15]=[C:14]([CH3:16])[C:13]([O:17][CH3:18])=[C:12]([CH3:19])[CH:11]=3)[O:20][C:6]=2[N:5]=[C:4]([S:22][CH3:23])[N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 24813Phosphorus oxychlorideHCID 516919Sodium BisulfateHCID 178490494HCID 178490494, 화합물

생성물 1

HCID 71743137HCID 71743137, 화합물

반응 조건

온도
70 °C

실험 절차

At room temperature, 45.95 g of N-(4,6-dihydroxy-2-methylsulfanylpyrimidin-5-yl)-4-methoxy-3,5-dimethylbenzamide were suspended with stirring in 125 ml of phosphorus oxychloride, and the mixture was heated at 70° C. for 36 hours. After cooling, the reaction mixture was sucked through a glass frit, giving a yellow solid which was introduced with stirring into a saturated aqueous sodium bisulfate solution and stirred for 10 min. The solid was then filtered off with suction, washed until neutral and dried. This gave 10.47 g (22%) of the title compound, which was reacted further without any further purification.

후처리

  1. customAt room temperature
  2. temperatureAfter cooling
  3. customgiving a yellow solid which
  4. additionwas introduced
  5. filtrationThe solid was then filtered off with suction
  6. washwashed until neutral and
  7. customdried
  8. customThis gave 10.47 g (22%) of the title compound, which was reacted further without any further purification

출처 및 근거

ORD 기록
ord-4d4e6f7453094fb29e3fd843d33eab93
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321787B2

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