Sodium Bicarbonate → 2-bromo-3-chloro-5H-pyrrolo[2,3-b]pyrazine

温度

0 °C

To a stirred solution of 5-bromo-6-chloro-3-trimethylsilanylethynyl-pyrazin-2-ylamine (2.0 g, 6.58 mmol) in THF (28 mL) was added a 1 M solution of KOtBu in THF (7.24 mL, 7.24 mmol) slowly at 0° C. under a nitrogen atmosphere. The reaction mixture was stirred at 0° C. for 10 min and then warmed to room temperature. After 2 h, the mixture was concentrated in vacuo and the residue obtained was suspended in water (7.5 mL) and saturated aqueous NaHCO3 (7.5 mL) and stirred overnight at room temperature The solid was filtered, washed with water and hexanes then dried in an oven at 80° C. to give 2-bromo-3-chloro-5H-pyrrolo[2,3-b]pyrazine (1.64 g) as brown solid. LC-MS: 232 (M−H). This was used directly without further purification.

1. temperaturewarmed to room temperature
2. waitAfter 2 h
3. concentrationthe mixture was concentrated in vacuo
4. customthe residue obtained
5. filtrationwas filtered
6. washwashed with water and hexanes
7. customthen dried in an oven at 80° C.

ORDレコード

ord-e8f33d4dadd64556a80205e3d01effdf

出典データセット

uspto-grants-2016_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09334278B2