Urea → HCID 178517410、化合物

反応式

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

参加物

反応物 2

HCID 1176Urea

HCID 235104752-Amino-5-bromobenzaldehyde

生成物 1

HCID 178517410HCID 178517410、化合物収率 89%

反応条件

温度: 180 °C

実験手順

A mixture of 2-amino-5-bromobenzaldehyde (29) (6 g, 30.0 mmol) and urea (30) (27 g, 450.0 mmol) was heated to 180° C. and stirred for 5 hours. LCMS showed the reaction was completed. The reaction mixture was cooled to room temperature, and the resulting precipitate was washed with H2O (3×500 mL) and co-evaporated with toluene three times to completely remove the moisture trapped. 6-bromoquinazolin-2-ol (31)(6 g, 89%) was obtained as a yellow solid. MS (ES+) C8H5BrN2O requires: 224. Found: 225, 227 [M+H]+.

後処理

temperatureThe reaction mixture was cooled to room temperature
washthe resulting precipitate was washed with H2O (3×500 mL) and co-evaporated with toluene three times
customto completely remove the moisture

出典と根拠

ORDレコード: ord-c300cde48c984cf3985abbcfe5ee9e40
出典データセット: uspto-grants-2015_09
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09126951B2

反応ノート

読み込み中…

参加物