Triethylamine → HCID 21086142, 화합물

HRID 349023

반응식

HRID 349023 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 21086142HCID 21086142, 화합물수율 82.7%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9d631dea45b54e34b64bd668616bdd5c
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07176242B2

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