Urea → 6-bromo-5-fluoroquinazolin-2(1H)-one

反応式

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

参加物

反応物 2

HCID 1176Urea

HCID 593253016-Amino-3-bromo-2-fluorobenzaldehyde

生成物 1

HCID 1785175476-bromo-5-fluoroquinazolin-2(1H)-one収率 99%

反応条件

温度: 180 °C

実験手順

A mixture of 6-amino-3-bromo-2-fluorobenzaldehyde (3.0 g, 13.76 mmol) and urea (12.40 g, 206.40 mmol) was heated to 180° C. and stirred for 2 hours. The reaction mixture was cooled to room temperature. The resulting precipitate was collected, washed with water (3×100 mL) and co-evaporated with toluene three times to completely remove the moisture trapped. The title compound (3.3 g, 99%) was obtained as a yellow solid. MS (ES+) C8H4BrFN2O requires: 242, found: 243, 245 [M+H]+.

後処理

temperatureThe reaction mixture was cooled to room temperature
customThe resulting precipitate was collected
washwashed with water (3×100 mL) and co-evaporated with toluene three times
customto completely remove the moisture

出典と根拠

ORDレコード: ord-3d8cf525cf674d158afa3669929b43d9
出典データセット: uspto-grants-2016_09
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09434700B2

反応ノート

読み込み中…

参加物