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Sodium Hydroxide → HCID 23708595、化合物

HRID 1379298
ノート
印刷プレビュー

反応式

HRID 1379298 の反応式
[F:1][C:2]([F:18])([F:17])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[C:4]=1[S:10]([O:13]C(C)C)(=[O:12])=[O:11].[OH-].[Na+:20]>O1CCCC1.O>[F:18][C:2]([F:1])([F:17])[C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([CH3:9])[C:4]=1[S:10]([O-:13])(=[O:11])=[O:12].[Na+:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 11832867Isopropyl 2-trifluoromethyl-6-methylbenzenesulfonate2 回

生成物 1

HCID 23708595HCID 23708595、化合物収率 92.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 83 g of the crude isopropyl 2-trifluoromethyl-6-methylbenzenesulfonate (which contained about 10% of isopropyl 2-trifluoromethylbenzenesulfonate) in 300 mL of tetrahydrofuran was treated with a solution of 24.8 g of 50% aqueous sodium hydroxide in 150 mL of water and heated to reflux for 4 hours, then stirred at room temperature overnight. The mixture was assayed by capillary GC (10 m DB-1, 100°-250° C. at 20° C./min) to ascertain that the isopropyl 2-trifluoromethyl-6-methylbenzenesulfonate was consumed. The tetrahydrofuran was removed in vacuo, then the remainder was poured into 100 mL of water and 200 mL of hexane. The aqueous phase was washed with hexane, then the water removed in vacuo to yield 71 g sodium 2-trifluoromethyl-6-methylbenzenesulfonate as a white solid.

後処理

  1. temperatureheated
  2. temperatureto reflux for 4 hours
  3. customwas assayed by capillary GC (10 m DB-1, 100°-250° C. at 20° C./min)
  4. customwas consumed
  5. customThe tetrahydrofuran was removed in vacuo
  6. additionthe remainder was poured into 100 mL of water and 200 mL of hexane
  7. washThe aqueous phase was washed with hexane
  8. customthe water removed in vacuo

出典と根拠

ORDレコード
ord-962d6d7eb17c4ecdaae6666ad10fedf5
出典データセット
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05670691

反応ノート

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