Phosphorus oxychloride → HCID 59312932, 화합물

HRID 2171476노트

반응식

HRID 2171476 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:14]=[C:13](O)[N:12]2[CH:16]=[CH:17][N:18]=[C:11]2[CH:10]=1.P(Cl)(Cl)([Cl:21])=O>C(=O)(O)[O-].[Na+]>[Cl:21][C:13]1[N:12]2[CH:16]=[CH:17][N:18]=[C:11]2[CH:10]=[C:9]([C:3]2[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=2[Cl:1])[N:14]=1

참가 물질

4

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178517482HCID 178517482, 화합물

생성물 1

HCID 59312932HCID 59312932, 화합물

시약·촉매·용매 1

HCID 516892Sodium Bicarbonate용매2회

반응 조건

온도
120 °C

실험 절차

12.0 g (42.84 mmol) of 7-(2,4-dichlorophenyl)imidazo[1,2-c]pyrimidin-5-ol are introduced into 131.6 g (858.27 mmol) of phosphoryl chloride and heated at 120° C. for 5 h. A clear solution is produced after 10 min. The mixture is allowed to cool, and then 2000 ml of saturated aqueous sodium bicarbonate solution are cautiously added. Towards the end, about 100 g of solid sodium bicarbonate are also added, and the mixture is stirred at pH 7 for 10 min. The precipitate is filtered off with suction, thoroughly washed with water, suspended in a little isopropanol and sucked dry. It is then washed once more with petroleum ether and dried under high vacuum at 50° C. 11 g (81% of theory) of the product are obtained as a solid.

후처리

  1. customA clear solution is produced after 10 min
  2. temperatureto cool
  3. filtrationThe precipitate is filtered off with suction
  4. washthoroughly washed with water
  5. customsucked dry
  6. washIt is then washed once more with petroleum ether
  7. customdried under high vacuum at 50° C
  8. custom11 g (81% of theory) of the product are obtained as a solid

출처 및 근거

ORD 기록
ord-cbe0d9db9b74465b92f58d3bcddaecbd
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09051323B2

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