Hydrochloric Acid → 3-(alpha,alpha,alpha,alpha',alpha',alpha'-Hexafluoro-3,5-Xylyl)-4,5-Isothiazoledicarboxylic Acid

HRID 614178ノート

反応式

HRID 614178 の反応式
[F:1][C:2]([F:27])([F:26])[C:3]1[CH:4]=[C:5]([C:13]2[C:17]([C:18]([O:20]C)=[O:19])=[C:16]([C:22]([O:24]C)=[O:23])[S:15][N:14]=2)[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.[OH-].[Na+].Cl>O>[F:12][C:9]([F:10])([F:11])[C:7]1[CH:6]=[C:5]([C:13]2[C:17]([C:18]([OH:20])=[O:19])=[C:16]([C:22]([OH:24])=[O:23])[S:15][N:14]=2)[CH:4]=[C:3]([C:2]([F:1])([F:27])[F:26])[CH:8]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 12437420Dimethyl 3-(alpha,alpha,alpha,alpha',alpha',alpha'-Hexafluoro-3,5-Xylyl)-4,5-Isothiazoledicarboxylate

生成物 1

HCID 124374403-(alpha,alpha,alpha,alpha',alpha',alpha'-Hexafluoro-3,5-Xylyl)-4,5-Isothiazoledicarboxylic Acid

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 14.7 g (0.0356 mol) of dimethyl 3-(α,α,α,α',α',α'-hexafluoro-3,5-xylyl)-4,5-isothiazoledicarboxylate, 7.2 g (0.18 mol) of NaOH, and 45 ml of water was held at reflux for 2 hours, was cooled, extracted twice with ether, and acidified with 30 ml (0.36 mol) of concentrated HCl The resultant mixture was extracted three times with ether; these ether extracts were combined, dried (CaSO4), and concentrated under vacuum to 12.8 g (93.4%) of white solid, m.p 193°-193.5° with decomposition.

後処理

  1. temperatureat reflux for 2 hours
  2. temperaturewas cooled
  3. extractionextracted twice with ether
  4. extractionwas extracted three times with ether
  5. dry with materialdried (CaSO4)
  6. concentrationconcentrated under vacuum to 12.8 g (93.4%) of white solid, m.p 193°-193.5° with decomposition

出典と根拠

ORDレコード
ord-6905dd68d3f441fb903a2f6bd54b4e74
出典データセット
uspto-grants-1979_03
特許番号
US04144047

反応ノート

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