Acetic Acid → 6-(Difluoromethoxy)[1]benzofuro[3,2-c]pyridine-9-carboxylic acid

HRID 1091868ノート

反応式

HRID 1091868 の反応式
C[O:2][C:3]([C:5]1[C:10]2[C:11]3[CH:12]=[N:13][CH:14]=[CH:15][C:16]=3[O:17][C:9]=2[C:8]([O:18][CH:19]([F:21])[F:20])=[CH:7][CH:6]=1)=[O:4].[OH-].[Na+].C(O)(=O)C>CO.O>[F:21][CH:19]([F:20])[O:18][C:8]1[C:9]2[O:17][C:16]3[CH:15]=[CH:14][N:13]=[CH:12][C:11]=3[C:10]=2[C:5]([C:3]([OH:4])=[O:2])=[CH:6][CH:7]=1

参加物

6

反応物 3

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 66592827Methyl-6-difluoromethyloxybenzo[4,5]furo[3,2-c]pyridine-9-carboxylate

生成物 1

HCID 593961556-(Difluoromethoxy)[1]benzofuro[3,2-c]pyridine-9-carboxylic acid収率 89.1%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒2 回

実験手順

A solution of Methyl-6-difluoromethyloxybenzo[4,5]furo[3,2-c]pyridine-9-carboxylate (6.5 g, 0.0221 moles), sodium hydroxide (4.0 g, 0.110 moles) and water (10.0 mL) in methanol (60.0 mL) was refluxed for 1-1.5 hrs. Methanol was removed under reduced pressure. The residue obtained was diluted with water (50.0 mL) and acidified with acetic acid. The solid separated was filtered, washed with water (2×100 mL) and dried to get 5.5 g of product as off-white solid.

後処理

  1. customMethanol was removed under reduced pressure
  2. customThe residue obtained
  3. customThe solid separated
  4. filtrationwas filtered
  5. washwashed with water (2×100 mL)
  6. customdried

出典と根拠

ORDレコード
ord-c52851c4782f45fe834b04214423076e
出典データセット
uspto-grants-2012_03
特許番号
US08129401B2

反応ノート

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