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

HRID 1189710노트

반응식

HRID 1189710 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
125 °C

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-dc5fa820f87644598b971facd31ebc4a
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08674136B2

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