Triethylamine → Methyl 5-bromopyrimidine-2-carboxylate

HRID 1011650

反応式

HRID 1011650 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 45790831Methyl 5-bromopyrimidine-2-carboxylate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-19c777ff27fe4c4f8e4625c32492bb88
出典データセット
uspto-grants-2011_07
特許番号
US07977372B2

関連ノート

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