Dichloromethane → HCID 178516729, 화합물

A pressure-resistant vessel was charged with 5-chloro-2-methoxypyrido[3,4-b]pyrazine (5.0 g, 26 mmol) and DCE (25 mL). To this was added a 1M solution of boron tribromide in dichloromethane (82 mL, 82 mmol) slowly via syringe. The vessel was sealed, and the reaction was stirred at ambient temperature overnight. After 16 hours, the reaction was quenched by slow addition of the reaction mixture into a beaker containing methanol (100 mL) and ice. The resulting yellow solution was concentrated to a tan slurry, which was triturated with ethyl acetate (50 mL). The off-white precipitate was collected by vacuum filtration, washed with ethyl acetate, and dried in vacuo to provide the title compound (7.2 g, 40 mmol, 155% yield) along with some bromide salts. LC/MS (ESI+) m/z: 182.1 (M+H+).

1. customThe vessel was sealed
2. waitAfter 16 hours
3. customthe reaction was quenched by slow addition of the reaction mixture into a beaker
4. additioncontaining methanol (100 mL) and ice
5. concentrationThe resulting yellow solution was concentrated to a tan slurry, which
6. customwas triturated with ethyl acetate (50 mL)
7. filtrationThe off-white precipitate was collected by vacuum filtration
8. washwashed with ethyl acetate
9. customdried in vacuo

ORD 기록

ord-b1d85059bf9d4a3090b22293dbddaa16

출처 데이터셋

uspto-grants-2016_04

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US09309263B2