Bromine → HCID 58431340, 화합물

HRID 1426309

반응식

HRID 1426309 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 24408Bromine2회HCID 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, the color of bromine was dissipated. The acetic acid was removed in vacuo and was followed by dissolving of the residue in toluene and removal of solvent in vacuo. The percent by weight of desired component in the mixture (containing unreacted starting material and overbrominated product) was determined by NMR and the mixture used without further purification (1.62 g, 61%). 1H NMR (300 MHz, CDCl3): δ 8.32 (s, 1H), 4.60 (s, 2H), 4.54 (q, 2H), 1.46 (t, 3H); LCMS (M+H)+: 313.0, 315.0

후처리

  1. customThe acetic acid was removed in vacuo
  2. dissolutionby dissolving of the residue in toluene
  3. customremoval of solvent in vacuo
  4. additionThe percent by weight of desired component in the mixture (containing unreacted starting material and overbrominated product)
  5. customthe mixture used without further purification (1.62 g, 61%)

출처 및 근거

ORD 기록
ord-0a72c58090a64fdbb1ebd67d96e5bb41
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08933085B2

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