Hydrochloric Acid → 3-Bromo-4-(hydroxymethyl)benzoic acid

HRID 594069

反応式

HRID 594069 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH2:11]Br)[C:5]([OH:7])=[O:6].Cl.[OH2:14]>CCOC(C)=O>[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[CH2:11][OH:14])[C:5]([OH:7])=[O:6]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 116163143-bromo-4-(bromomethyl)benzoic Acid

生成物 1

HCID 196884153-Bromo-4-(hydroxymethyl)benzoic acid

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
95 °C

実験手順

To a solution of yield 3-bromo-4-(bromomethyl)benzoic acid (1.0 equiv.) in Water (0.56 M) at 95° C. was added potassium carbonate K2CO3 (5.0 equiv.). The homogenous reaction mixture was stirred at 95° C. in an oil bath for 1 hr. The reaction mixture was COOLED OFF TO RT, neutralized with 6 M HCl. diluted with EtOAc and washed with brine. The organic layer was dried over Na2SO4, filtered and concentrated. The crude was used in next step. LC/MS (m/z)=294.8 (MH+), Rt=0.80 min.

後処理

  1. temperatureThe reaction mixture was COOLED OFF TO RT
  2. washwashed with brine
  3. dry with materialThe organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-2ce244944b804f83b89469331bd59216
出典データセット
uspto-grants-2016_01
特許番号
US09242969B2

関連ノート

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