Triethylamine → Methyl 5-bromopyrimidine-2-carboxylate

HRID 1011650

반응식

HRID 1011650 반응식
[Br:1][C:2]1[CH:3]=[N:4][C:5]([C:8]([OH:10])=[O:9])=[N:6][CH:7]=1.[CH3:11]CN(CC)CC.S(Cl)(Cl)(=O)=O>CO>[CH3:11][O:9][C:8]([C:5]1[N:6]=[CH:7][C:2]([Br:1])=[CH:3][N:4]=1)=[O:10]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 24648Sulfuryl chlorideHCID 164629705-Bromopyrimidine-2-carboxylic acid

생성물 1

HCID 45790831Methyl 5-bromopyrimidine-2-carboxylate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 5-bromo-2-pyrimidine carboxylic acid (6 g, 29.6 mmol) in MeOH (300 mL) was added Et3N (5.98 g, 59.2 mmol). The mixture was cooled to 0 degrees Celsius, and sulfonyl chloride (5.3 g, 44.4 mmol) was added dropwise to the solution. After addition, the mixture was stirred at rt for 12 hours. The solvent was removed and the residue was dissolved in ethyl acetate. The organic layer was washed with sodium bicarbonate, brine, and dried with sodium sulfate. The solvent was removed to give the pure product. MS: calc'd 217 (MH+), exp 217 (MH+).

후처리

  1. temperatureThe mixture was cooled to 0 degrees Celsius
  2. additionAfter addition
  3. customThe solvent was removed
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. washThe organic layer was washed with sodium bicarbonate, brine
  6. dry with materialdried with sodium sulfate
  7. customThe solvent was removed
  8. customto give the pure product

출처 및 근거

ORD 기록
ord-19c777ff27fe4c4f8e4625c32492bb88
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07977372B2

연결된 노트

불러오는 중…