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

HRID 1409496ノート

反応式

HRID 1409496 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 RTovernight. 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-2773c11f09c444dcbbe5000044a65642
出典データセット
uspto-grants-2014_12
特許番号
US08921363B2

反応ノート

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