Sulfuric Acid → 6-Bromo-4-chloropyrrolo[1,2-b]pyridazine-3-carboxamide

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[Br:1][C:2]1[CH:3]=[C:4]2[C:9]([Cl:10])=[C:8]([C:11]#[N:12])[CH:7]=[N:6][N:5]2[CH:13]=1.[OH:14]S(O)(=O)=O>>[Br:1][C:2]1[CH:3]=[C:4]2[C:9]([Cl:10])=[C:8]([C:11]([NH2:12])=[O:14])[CH:7]=[N:6][N:5]2[CH:13]=1

참가 물질

반응물 2

HCID 1118Sulfuric Acid

HCID 682911366-Bromo-4-chloropyrrolo[1,2-b]pyridazine-3-carbonitrile

생성물 1

HCID 682911926-Bromo-4-chloropyrrolo[1,2-b]pyridazine-3-carboxamide수율 89%

반응 조건

온도: 55 °C

실험 절차

To a 50 mL round bottom flask was added 6-bromo-4-chloropyrrolo[1,2-b]pyridazine-3-carbonitrile (12 g, 0.046 mol) and concentrated H2SO4 (60 mL). The reaction mixture was heated at 55° C. for 2 hours then cooled to room temperature and slowly diluted with ice water to precipitate the product which was collected by vacuum filtration, rinsed with water and dried to yield 11.2 g (89%) of the title compound as a yellow solid. HPLC (condition P): retention time=7.780 min.

후처리

temperaturethen cooled to room temperature
customto precipitate the product which
filtrationwas collected by vacuum filtration
washrinsed with water
customdried

출처 및 근거

ORD 기록: ord-8c2f9e28f7d247b9a939faf2f6b2cce7
출처 데이터셋: uspto-grants-2015_12
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09221826B2

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