Dimethylformamide dimethyl acetal → HCID 178484240, 화합물

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

참가 물질

반응물 2

HCID 78373Dimethylformamide dimethyl acetal

HCID 27947796-Bromopyridazin-3-amine

생성물 1

HCID 178484240HCID 178484240, 화합물수율 74.5%

실험 절차

3-Amino-6-bromopyridazine (5.0 g, 28.7 mmol) was heated and stirred with dimethylformamide dimethylacetal (5.36 g, 6.0 mL, 45.0 mmol) under nitrogen at 110° C. for 3 h. The brown homogeneous reaction mixture was cooled to room temperature. The resulting heterogeneous slurry was stirred in EtOAc/hexanes (1:1, 75 mL) and filtered. The filtered solid was suction dried to obtain apparently (E)-N′-(6-bromopyridazin-3-yl)-N,N-dimethylformimidamide (4.9 g) as a pale pink crystalline solid. 1H NMR (300 MHz, DMSO-d6) δ 8.45 (s, 1H), 7.64 (d, J=9.1 Hz, 1H), 7.03 (d, J=9.1 Hz, 1H), 3.11 (s, 3H), 3.00 (s, 3H).

후처리

filtrationfiltered
customdried

출처 및 근거

ORD 기록: ord-3a6bfbd691de477abcfc45c000071a63
출처 데이터셋: uspto-grants-2015_09
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09145433B2

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