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

HRID 529419ノート

反応式

HRID 529419 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 stiffed 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-37add0afa81a470c9c8135b2d4b116be
出典データセット
uspto-grants-2016_05
特許番号
US09346827B2

反応ノート

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