Lithium → 7,8-Difluoro-3,4-dihydro-2H-1,4-benzothiazine

HRID 2270240ノート

反応式

HRID 2270240 の反応式
[F:1][C:2]1[CH:12]=[CH:11][C:5]2[NH:6][C:7](=O)[CH2:8][S:9][C:4]=2[C:3]=1[F:13].[Li]>C1COCC1>[F:1][C:2]1[CH:12]=[CH:11][C:5]2[NH:6][CH2:7][CH2:8][S:9][C:4]=2[C:3]=1[F:13]

参加物

4

反応物 2

HCID 3028194LithiumHCID 22632969HCID 22632969、化合物

生成物 1

HCID 226329587,8-Difluoro-3,4-dihydro-2H-1,4-benzothiazine収率 104%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 7,8-difluoro-4H-benzo[1,4]thiazin-3-one (Example L-3, 2.27 g, 11.3 mmol) in THF (100 mL) was reacted with lithium aluminumhydride (1.07 g, 28.2 mmol) under an N2 atmosphere and heated to reflux overnight. The mixture was cooled and quenched with 1.0N HCl and extracted with ethyl acetate. The organic layers were combined, dried with sodium sulfate, and concentrated to provide 2.2 g of the title compound as an oil.

後処理

  1. temperatureheated
  2. temperatureto reflux overnight
  3. temperatureThe mixture was cooled
  4. customquenched with 1.0N HCl
  5. extractionextracted with ethyl acetate
  6. dry with materialdried with sodium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-141264a054654015bef40aa052e94ffa
出典データセット
uspto-grants-2001_12
特許番号
US06331538B1

反応ノート

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