Triethylamine → HCID 21086142、化合物

HRID 349023

反応式

HRID 349023 の反応式
Cl[C:2]1[N:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[CH:5]=[C:4]([CH3:12])[N:3]=1.[CH2:13]([NH:16][CH2:17][CH2:18][CH3:19])[CH2:14][CH3:15].C(N(CC)CC)C>C1COCC1>[CH2:13]([N:16]([CH2:17][CH2:18][CH3:19])[C:2]1[N:7]=[C:6]([C:8]([O:10][CH3:11])=[O:9])[CH:5]=[C:4]([CH3:12])[N:3]=1)[CH2:14][CH3:15]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 8902DipropylamineHCID 2736835Methyl 2-chloro-6-methylpyrimidine-4-carboxylate

生成物 1

HCID 21086142HCID 21086142、化合物収率 82.7%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of methyl 2-chloro-6-methylpyrimidine-4-carboxylate (0.411 g, 2.20 mmol), di-n-propylamine (0.668 g, 6.60 mmol), triethylamine (0.267 g, 2.64 mmol), and THF (5 ml) was stirred at room temperature for 55 min and then at reflux for 1.3 h, at which time is was cooled and partitioned between ethyl acetate and a mixture of brine and aq. sodium bicarbonate. The organic layer was dried over magnesium sulfate and concentrated and then chromatographed on silica gel using ethyl acetate-hexane (90/10) to give methyl 2-(dipropylamino)-6-methylpyrimidine-4-carboxylate (0.457 g) as a pale yellow liquid.

後処理

  1. temperatureat reflux for 1.3 h, at which time
  2. temperatureis was cooled
  3. custompartitioned between ethyl acetate
  4. additiona mixture of brine and aq. sodium bicarbonate
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. concentrationconcentrated
  7. customchromatographed on silica gel

出典と根拠

ORDレコード
ord-9d631dea45b54e34b64bd668616bdd5c
出典データセット
uspto-grants-2007_02
特許番号
US07176242B2

関連ノート

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