Bromine → HCID 58431340, 화합물

HRID 1617414

반응식

HRID 1617414 반응식
[CH3:1][C:2]1[N:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[N:5]=[C:4]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:3]=1.[Br:17]Br>C(O)(=O)C>[Br:17][CH2:1][C:2]1[N:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[N:5]=[C:4]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:3]=1

참가 물질

4

반응물 2

HCID 24408BromineHCID 67390769Ethyl 6-methyl-2-(trifluoromethyl)pyrimidine-4-carboxylate

생성물 1

HCID 58431340HCID 58431340, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
80 °C

실험 절차

A solution of ethyl 6-methyl-2-(trifluoromethyl)pyrimidine-4-carboxylate (2.00 g, 8.54 mmol, prepared as described in WO2007/090748) in acetic acid (12 mL) was treated with bromine (1.36 g, 8.54 mmol) and the reaction was heated to 80° C. in a sealed vial for 30 minutes, at which time it was decolorized. The mixture containing unreacted starting material, desired product, and over brominated product, was rotovapped and azeotroped once with toluene. The percent by weight of desired component was determined by NMR and the mixture used without further purification. Yield: 1.62 g (61%); LC-MS: 313.0, 315.0 (M+H)+. 1H NMR (300 MHz, CDCl3): δ 8.32 (s, 1H), 4.60 (s, 2H), 4.54 (q, 2H), 1.46 (t, 3H).

후처리

  1. additionThe mixture containing unreacted

출처 및 근거

ORD 기록
ord-43879bc991a245a8aa8a2f1ed1fbdc23
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08765734B2

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