Acetic Acid → 2-Naphthalenecarboxylic acid, 7-bromo-3-hydroxy-

HRID 1189710ノート

反応式

HRID 1189710 の反応式
Br[C:2]1[C:11]2[C:6](=[CH:7][C:8]([Br:12])=[CH:9][CH:10]=2)[CH:5]=[C:4]([C:13]([OH:15])=[O:14])[C:3]=1[OH:16].C(O)(=O)C.[Sn].Cl>O>[Br:12][C:8]1[CH:7]=[C:6]2[C:11]([CH:2]=[C:3]([OH:16])[C:4]([C:13]([OH:15])=[O:14])=[CH:5]2)=[CH:10][CH:9]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 745022-Naphthalenecarboxylic acid, 4,7-dibromo-3-hydroxy-HCID 5352426Tin atom

生成物 1

HCID 745032-Naphthalenecarboxylic acid, 7-bromo-3-hydroxy-収率 96.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
125 °C

実験手順

In a 1 L three-necked bottle, 40 g of 4,7-dibromo-3-hydroxy-2-naphthoic acid (0.116 mol) and 500 ml of glacial acetic acid were added, and stirred to make homogenous. 18 g of tin powder (0.153 mol) and 130 ml of concentrated hydrochloric acid were then added to the mixture in order, heated to 125° C., and refluxed under heating for 12 h. 300 ml of water was added to the mixture, stirred to room temperature, filtered, and the filter cake was washed with water (200 ml*2), and dried in an oven to obtain 29.9 g of a solid with a yield of 96.5%.

後処理

  1. temperaturerefluxed
  2. temperatureunder heating for 12 h
  3. stirringstirred to room temperature
  4. filtrationfiltered
  5. washthe filter cake was washed with water (200 ml*2)
  6. customdried in an oven

出典と根拠

ORDレコード
ord-dc5fa820f87644598b971facd31ebc4a
出典データセット
uspto-grants-2014_03
特許番号
US08674136B2

反応ノート

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