Isopropanol → Isopropyl 2-Chloro-4-Trifluoromethyl-5-Thiazolecarboxylate

HRID 1413642ノート

反応式

HRID 1413642 の反応式
[Cl:1][C:2]1[S:3][C:4]([C:11](Cl)=[O:12])=[C:5]([C:7]([F:10])([F:9])[F:8])[N:6]=1.[CH:14]([OH:17])([CH3:16])[CH3:15]>>[Cl:1][C:2]1[S:3][C:4]([C:11]([O:17][CH:14]([CH3:16])[CH3:15])=[O:12])=[C:5]([C:7]([F:8])([F:9])[F:10])[N:6]=1

参加物

3

反応物 2

HCID 3776IsopropanolHCID 132827442-Chloro-4-trifluoromethyl-5-thiazolecarbonyl chloride

生成物 1

HCID 13282745Isopropyl 2-Chloro-4-Trifluoromethyl-5-Thiazolecarboxylate収率 86.1%

実験手順

The acid chloride of Example 8 (5.2 g), and 10 g of isopropanol were held at reflux for 16 hours. Excess alcohol was removed under reduced pressure. The residue was dissolved in 50 ml. of ether. The ether solution was washed with sodium bicarbonate, dried (MgSO4) and concentrated under reduced pressure. The crude product was distilled at 1 mm. on a Kugelrohr to give 4.9 g (86%) of the desired product as colorless liquid, nD25 =1.4655.

後処理

  1. temperatureat reflux for 16 hours
  2. customExcess alcohol was removed under reduced pressure
  3. dissolutionThe residue was dissolved in 50 ml
  4. washThe ether solution was washed with sodium bicarbonate
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated under reduced pressure
  7. distillationThe crude product was distilled at 1 mm

出典と根拠

ORDレコード
ord-dde1fca615f14bff9fcb389d41a2bd89
出典データセット
uspto-grants-1981_02
特許番号
US04251261

反応ノート

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