1,8-Diazabicyclo(5.4.0)undec-7-ene → 4H-Pyrano(2,3-b)pyridine, 6-bromo-2-(3,4-dichlorophenyl)-

HRID 280192ノート

反応式

HRID 280192 の反応式
[Br:1][C:2]1[CH:3]=[C:4]2[CH:11]=[CH:10][CH:9]([C:12]3[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([Cl:19])[CH:13]=3)[O:8][C:5]2=[N:6][CH:7]=1.N12CCCN=C1CCCCC2>O1CCCC1>[Br:1][C:2]1[CH:3]=[C:4]2[CH2:11][CH:10]=[C:9]([C:12]3[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([Cl:19])[CH:13]=3)[O:8][C:5]2=[N:6][CH:7]=1

参加物

4

反応物 2

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 5149096-bromo-2-(3,4-dichlorophenyl)-2H-pyrano[2,3-b]pyridine

生成物 1

HCID 5149104H-Pyrano(2,3-b)pyridine, 6-bromo-2-(3,4-dichlorophenyl)-

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 2.9 g of 6-bromo-2-(3,4-dichlorophenyl)-2H-pyrano[2,3-b]pyridine in 40 ml of tetrahydrofuran was added 0.5 ml of 1,8-diazabicyclo[5.4.0]undec-7-ene. After 1 hour at 25° C., the reaction mixture was partitioned between ethyl acetate and aqueous saturated ammonium chloride solution. The ethyl acetate layer was dried over magnesium sulfate and the solvent was evaporated to leave a solid residue. This was recrystallized from ethanol to give 6-bromo-2-(3,4-dichlorophenyl)-4H-pyrano[2,3-b]pyridine melting at about 138°-139.5° C.

後処理

  1. customthe reaction mixture was partitioned between ethyl acetate and aqueous saturated ammonium chloride solution
  2. dry with materialThe ethyl acetate layer was dried over magnesium sulfate
  3. customthe solvent was evaporated
  4. customto leave a solid residue
  5. customThis was recrystallized from ethanol

出典と根拠

ORDレコード
ord-eafa897dc1514dfeadaa3a24cf00cebe
出典データセット
uspto-grants-1986_05
特許番号
US04588733

反応ノート

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