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

HRID 2270240노트

반응식

HRID 2270240 반응식
[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]

참가 물질

4

반응물 2

HCID 3028194LithiumHCID 22632969HCID 22632969, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-141264a054654015bef40aa052e94ffa
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06331538B1

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