Dimethylformamide diethylacetal → Ethyl 3-(dimethylamino)-2-(1H-1,2,3-triazol-1-yl)acrylate

반응식

C(O[CH:4](OCC)[N:5]([CH3:7])[CH3:6])C.[N:11]1([CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])[CH:15]=[CH:14][N:13]=[N:12]1>>[CH3:4][N:5]([CH3:7])[CH:6]=[C:16]([N:11]1[CH:15]=[CH:14][N:13]=[N:12]1)[C:17]([O:19][CH2:20][CH3:21])=[O:18]

참가 물질

반응물 2

HCID 70913Dimethylformamide diethylacetal

HCID 10103365Ethyl 2-(1H-1,2,3-triazol-1-YL)acetate

생성물 1

HCID 66726233Ethyl 3-(dimethylamino)-2-(1H-1,2,3-triazol-1-yl)acrylate

반응 조건

온도: 100 °C

실험 절차

44.2 ml (38.0 g, 257.8 mmol) of N,N-dimethylformamide diethyl acetal are added to 20.0 g (128.9 mmol) of the compound from Example 2A, and the mixture is stirred at 100° C. for 16 h. After cooling to RT, the reaction mixture is concentrated under reduced pressure. The residue is triturated with diethyl ether, filtered off and washed with diethyl ether. Yield: 18.0 g (67% of theory)

후처리

temperatureAfter cooling to RT
concentrationthe reaction mixture is concentrated under reduced pressure
customThe residue is triturated with diethyl ether
filtrationfiltered off
washwashed with diethyl ether

출처 및 근거

ORD 기록: ord-00e041146182450b850d5077fcfcfa55
출처 데이터셋: uspto-grants-2011_11
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08067407B2

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