Anthranilic Acid → HCID 19974595、化合物

HRID 1451640ノート

反応式

HRID 1451640 の反応式
Cl[C:2]1[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[C:13]([OH:22])(=[O:21])[C:14]1[C:15](=[CH:17][CH:18]=[CH:19][CH:20]=1)[NH2:16].C(=O)([O-])[O-].[K+].[K+].O>COCCOCCO.[Cu]>[C:13]([C:14]1[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=1[NH:16][C:2]1[CH:10]=[CH:9][C:8]([S:11][CH3:12])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5])([OH:22])=[O:21]

参加物

7

反応物 4

HCID 227Anthranilic AcidHCID 962WaterHCID 11430Potassium CarbonateHCID 6088142-Chloro-5-(methylsulfanyl)benzoic acid

生成物 1

HCID 19974595HCID 19974595、化合物収率 30.1%

試薬・触媒・溶媒 2

HCID 23978Copper触媒HCID 8134Diethylene Glycol Monomethyl Ether溶媒

実験手順

A mixture of 2-chloro-5-(methylthio)benzoic acid (10 g), anthranilic acid (7 g), potassium carbonate (14 g) and copper (1 g) in 2-(2-methoxyethoxy)ethanol (100 ml) was heated at 180° for 24 h. Water (400 ml) was then added, and the catalyst was filtered off. The filtrate was acidified with dilute hydrochloric acid. The resulting precipitate was filtered off, washed with water, dried, and crystallised from methanol to give the title compound (4.5 g) as crystals. IR includes peaks at 3300 cm-1 (NH) and 1700 cm-1 (CO2H).

後処理

  1. temperaturewas heated at 180° for 24 h
  2. filtrationthe catalyst was filtered off
  3. filtrationThe resulting precipitate was filtered off
  4. washwashed with water
  5. customdried
  6. customcrystallised from methanol

出典と根拠

ORDレコード
ord-e5607978b25d4d04a49c679fdfc77762
出典データセット
uspto-grants-1997_02
特許番号
US05604237

反応ノート

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