Dimethylformamide → 8-bromo-2-chloro-10H-chromeno[3,2-b]pyridin-10-one

HRID 1855289ノート

反応式

HRID 1855289 の反応式
[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[O:12][C:11]3[C:6](=[N+:7]([O-])[CH:8]=[CH:9][CH:10]=3)[C:5](=[O:17])[C:4]=2[CH:3]=1.P(Cl)(Cl)([Cl:20])=O.CN(C=O)C>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:15]=[CH:14][C:13]2[O:12][C:11]3[C:6](=[N:7][C:8]([Cl:20])=[CH:9][CH:10]=3)[C:5](=[O:17])[C:4]=2[CH:3]=1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 667282008-bromo-10-oxo-10H-chromeno[3,2-b]pyridine 1-oxide

生成物 1

HCID 584661968-bromo-2-chloro-10H-chromeno[3,2-b]pyridin-10-one

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a suspension of 8-bromo-10-oxo-10H-chromeno[3,2-b]pyridine 1-oxide in 100 mL of toluene at 0° C. was added dropwise phosphorus oxychloride (35.8 mL, 391 mmol) followed by 2 mL of DMF and the mixture was stirred at RT overnight. The solvent was evaporated under vacuum and the residue which crashed out of water, was filtered and washed with water, methanol and acetone in sequence. The solid was air dried to give 8-bromo-2-chloro-10H-chromeno[3,2-b]pyridin-10-one as a tan solid.

後処理

  1. customThe solvent was evaporated under vacuum
  2. filtrationwas filtered
  3. washwashed with water, methanol and acetone in sequence
  4. customdried

出典と根拠

ORDレコード
ord-32f67db33ea848779b6b6e3600865932
出典データセット
uspto-grants-2015_02
特許番号
US08962859B2

反応ノート

読み込み中…