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Phosphorus oxychloride → HCID 59313005, 화합물

HRID 2171550
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HRID 2171550 반응식
O[C:2]1[N:7]2[N:8]=[C:9]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[N:10]=[C:6]2[CH:5]=[C:4]([C:16]2[CH:21]=[CH:20][C:19]([C:22]([F:25])([F:24])[F:23])=[CH:18][CH:17]=2)[N:3]=1.P(Cl)(Cl)([Cl:28])=O>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.C(=O)(O)[O-].[Na+]>[Cl:28][C:2]1[N:7]2[N:8]=[C:9]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[N:10]=[C:6]2[CH:5]=[C:4]([C:16]2[CH:21]=[CH:20][C:19]([C:22]([F:25])([F:24])[F:23])=[CH:18][CH:17]=2)[N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 24813Phosphorus oxychlorideHCID 178470152HCID 178470152, 화합물

생성물 1

HCID 59313005HCID 59313005, 화합물

시약·촉매·용매 2

HCID 66133Benzyl triethylammonium chloride촉매HCID 516892Sodium Bicarbonate용매2회

반응 조건

온도
120 °C

실험 절차

2300 mg (6.5 mmol) of ethyl 5-hydroxy-7-[4-(trifluoromethyl)phenyl][1,2,4]triazolo-[1,5-c]pyrimidine-2-carboxylate (Example 133A) are introduced into phosphoryl chloride (30 ml), 5.95 g (26.1 mmol) of benzyltriethylammonium chloride are added, and the reaction mixture is stirred at 120° C. for 20 h. The reaction mixture is slowly poured, while stirring vigorously, into saturated sodium bicarbonate solution (200 ml) and ice, and solid sodium bicarbonate (approx. 20 g) is added until a pH of 8 is reached. The solid is filtered off with suction and washed with water and diethyl ether and dried. 2300 mg (92% of theory) of the product are obtained.

후처리

  1. additionare added
  2. additionThe reaction mixture is slowly poured
  3. additionis added until a pH of 8
  4. filtrationThe solid is filtered off with suction
  5. washwashed with water and diethyl ether
  6. customdried
  7. custom2300 mg (92% of theory) of the product are obtained

출처 및 근거

ORD 기록
ord-7d8bae4574b34c5f93b803107daf2192
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09051323B2

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