Hydrochloric Acid → 4-(4-Bromo-3-formylphenoxy)-3-hydroxybenzonitrile

HRID 1471481ノート

反応式

HRID 1471481 の反応式
[Br:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:14]=[CH:13][C:10]([C:11]#[N:12])=[CH:9][C:8]=2[O:15]COC)=[CH:4][C:3]=1[CH:21]1OCC[O:22]1.Cl.O>O1CCCC1>[Br:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:14]=[CH:13][C:10]([C:11]#[N:12])=[CH:9][C:8]=2[OH:15])=[CH:4][C:3]=1[CH:21]=[O:22]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 674390784-(4-Bromo-3-(1,3-dioxolan-2-yl)phenoxy)-3-methoxymethoxybenzonitrile

生成物 1

HCID 866364134-(4-Bromo-3-formylphenoxy)-3-hydroxybenzonitrile収率 102.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 4-(4-bromo-3-(1,3-dioxolan-2-yl)phenoxy)-3-methoxymethoxybenzonitrile (32.2 g, 79.3 mmol) in tetrahydrofuran (300 mL) was added 3 M HCl (100 mL), and the mixture was refluxed for 2 h. Water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine and dried on anhydrous sodium sulfate. The solvent was removed under reduced pressure to give 4-(4-bromo-3-formylphenoxy)-3-hydroxybenzonitrile (25.8 g, quant.).

後処理

  1. temperaturethe mixture was refluxed for 2 h
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with brine
  4. dry with materialdried on anhydrous sodium sulfate
  5. customThe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-632ebcd143844b74a3fcc1fc53976df2
出典データセット
uspto-grants-2015_04
特許番号
US09012431B2

反応ノート

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