6-Amino-3-chloropyridazine → HCID 178484245, 화합물

반응식

[Cl:1][C:2]1[N:7]=[N:6][C:5]([NH2:8])=[CH:4][CH:3]=1.CO[CH:11](OC)[N:12]([CH3:14])[CH3:13]>>[Cl:1][C:2]1[N:7]=[N:6][C:5](/[N:8]=[CH:11]/[N:12]([CH3:14])[CH3:13])=[CH:4][CH:3]=1

참가 물질

반응물 2

HCID 216436-Amino-3-chloropyridazine

HCID 78373Dimethylformamide dimethyl acetal

생성물 1

HCID 178484245HCID 178484245, 화합물수율 82.9%

반응 조건

온도: 110 °C

실험 절차

A 500 mL RB flask was charged with 6-chloropyridazin-3-amine (10.0 g, 77.2 mmol) and dimethoxy-N,N-dimethylmethanamine (206 ml, 1544 mmol), equipped with a reflux condenser, then heated to 110° C. for 3 hours then left at room temperature for 16 hours. The precipitate was collected by filtration. The mother liqour was concentrated down to give an yellow solid, which was triturated with EtOAc and collected. The solids were combined to give (E)-N′-(6-chloropyridazin-3-yl)-N,N-dimethylformamidine (11.81 g, 82.9% yield) as a white solid

후처리

customequipped with a reflux condenser
filtrationThe precipitate was collected by filtration
concentrationThe mother liqour was concentrated down
customto give an yellow solid, which
customwas triturated with EtOAc
customcollected

출처 및 근거

ORD 기록: ord-f47ed11a07204948b95a84095b32d6f5
출처 데이터셋: uspto-grants-2013_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US08524900B2

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