Water → 3,6-Dichloro-2-methoxybenzohydroxamic acid

HRID 568741

反応式

HRID 568741 の反応式
C(=O)([O-])[O-].[K+].[K+].[OH2:7].Cl.[NH2:9]O.[Cl:11][C:12]1[C:13]([O:22][CH3:23])=[C:14]([C:18]([Cl:21])=[CH:19][CH:20]=1)[C:15](Cl)=[O:16]>C(OCC)C>[Cl:11][C:12]1[C:13]([O:22][CH3:23])=[C:14]([C:18]([Cl:21])=[CH:19][CH:20]=1)[C:15]([NH:9][OH:7])=[O:16]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 82609Benzoyl chloride, 3,6-dichloro-2-methoxy-HCID 443297Hydroxyamine hydrochloride

生成物 1

HCID 140973413,6-Dichloro-2-methoxybenzohydroxamic acid

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To a solution of 360 g. of potassium carbonate in 350 ml. of water was added 2.5 diethyl ether and 181 g. hydroxylamine hydrochloride. The mixture was cooled to 5°-1O° C. and 477 g. of 3,6-dichloro-2-methoxybenzoyl chloride was added dropwise at a rate that maintained the reaction temperature below 10° C. After addition was complete, the reaction mixture was stirred for 1 hour and allowed to stand overnight at ambient temperature. The crude white solid product was obtained by filtration. The crude solid was washed with water, then treated with 1.5 of 4.5 M. HCl, filtered, washed again with H2O and dried to give 3,6-dichloro-2-methoxybenzohydroxamic acid as a white solid, m.p. 150° C.

後処理

  1. temperatureThe mixture was cooled to 5°-1O° C
  2. temperaturemaintained the reaction temperature below 10° C
  3. additionAfter addition
  4. waitto stand overnight at ambient temperature
  5. customThe crude white solid product was obtained by filtration
  6. washThe crude solid was washed with water
  7. additiontreated with 1.5 of 4.5 M
  8. filtrationHCl, filtered
  9. washwashed again with H2O
  10. customdried

出典と根拠

ORDレコード
ord-7c172a25a7d3423c8880c15efb992580
出典データセット
uspto-grants-1988_03
特許番号
US04729781

関連ノート

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