Nitrogen → 7-bromo-3-fluoro-2-methoxy-9H-xanthen-9-one

HRID 335917

反応式

HRID 335917 の反応式
N#N.OS(O)(=O)=O.[Br:8][C:9]1[CH:27]=[CH:26][C:12]([O:13][C:14]2[CH:22]=[C:21]([F:23])[C:20]([O:24][CH3:25])=[CH:19][C:15]=2[C:16]([OH:18])=O)=[CH:11][CH:10]=1>>[Br:8][C:9]1[CH:10]=[C:11]2[C:12]([O:13][C:14]3[CH:22]=[C:21]([F:23])[C:20]([O:24][CH3:25])=[CH:19][C:15]=3[C:16]2=[O:18])=[CH:26][CH:27]=1

参加物

4

反応物 3

HCID 947NitrogenHCID 1118Sulfuric AcidHCID 67383032HCID 67383032、化合物

生成物 1

HCID 584662337-bromo-3-fluoro-2-methoxy-9H-xanthen-9-one

反応条件

温度
60 °C

実験手順

A 3 neck 22 L RBF equipped with a mechanical stirrer, temperature probe and N2 inlet was charged with concentrated H2SO4 (2.7 L) and heated to 60° C. To this mixture was added 2-(4-bromophenoxy)-4-fluoro-5-methoxybenzoic acid (1.3 kg, 3.81 mol) in portions such that the internal temp remained below 70° C. The resulting mixture was stirred at 60° C. for 1 hour at which point the reaction mixture was cooled to 0° C. and slowly poured onto ice water. The resulting solids were removed by filtration, washed with water and triturated with EtOAc (3 L). The solid was then washed with EtOAc, hexane and dried under vacuum at 30° C. to afford 7-bromo-3-fluoro-2-methoxy-9H-xanthen-9-one as an off white solid.

後処理

  1. customA 3 neck 22 L RBF equipped with a mechanical stirrer
  2. customremained below 70° C
  3. temperaturewas cooled to 0° C.
  4. additionslowly poured onto ice water
  5. customThe resulting solids were removed by filtration
  6. washwashed with water
  7. customtriturated with EtOAc (3 L)
  8. washThe solid was then washed with EtOAc, hexane
  9. customdried under vacuum at 30° C.

出典と根拠

ORDレコード
ord-cfb04d01f6fe43b281519cb09a1c7e68
出典データセット
uspto-grants-2014_11
特許番号
US08883782B2

関連ノート

読み込み中…