HCID 86628018、化合物 → 8-Bromo-6-chloro-2H-1-benzopyran-2-one

HRID 2233327ノート

反応式

HRID 2233327 の反応式
[Br:1][C:2]1[C:3]([OH:15])=[C:4](/[CH:9]=[CH:10]/[C:11]([O:13]C)=O)[CH:5]=[C:6]([Cl:8])[CH:7]=1>C1C2C(CCCC2)CCC1>[Br:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]2[C:3]=1[O:15][C:11](=[O:13])[CH:10]=[CH:9]2

参加物

3

反応物 1

HCID 86628018HCID 86628018、化合物

生成物 1

HCID 187215758-Bromo-6-chloro-2H-1-benzopyran-2-one収率 95%

試薬・触媒・溶媒 1

HCID 7044Decalin溶媒

実験手順

A solution of methyl (2E)-3-(3-bromo-5-chloro-2-hydroxyphenyl)-2-propenoate (1.45 g; 5.0 mmol) in decalin (5 mL) was heated in a sand bath at 200° C. for 48 h. The reaction was then cooled to RT and hexanes (10 mL) was added. The solid was collected by suction filtration and washed with hexanes. Drying under high vacuum gave the title compound (1.2 g, 95%) as a tan solid: 1H NMR (400 MHz, DMSO-d6) δ 7.78 (s, 1H), 7.63 (d, J=9.6 Hz, 1H)), 7.46 (s, 1H), 6.52 (d, J=9.6 Hz, 1H); MS (ES) m/e 259, 261 (M+H)+.

後処理

  1. filtrationThe solid was collected by suction filtration
  2. washwashed with hexanes
  3. customDrying under high vacuum

出典と根拠

ORDレコード
ord-ae449f223cad4c949e91e431095a06b8
出典データセット
uspto-grants-2010_05
特許番号
US07709496B2

反応ノート

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