Nitric Acid → Thiomorpholine, 4-(2,6-difluoro-4-nitrophenyl)-, 1,1-dioxide

HRID 395261

반응식

HRID 395261 반응식
[O:1]=[S:2]1(=[O:27])[CH2:7][CH2:6][N:5]([C:8]2[C:13]([F:14])=[CH:12][C:11](N3C[C@H](CNC(=O)C)OC3=O)=[CH:10][C:9]=2[F:26])[CH2:4][CH2:3]1.[N+:28]([O-:31])(O)=[O:29].O>C(O)(=O)C>[F:14][C:13]1[CH:12]=[C:11]([N+:28]([O-:31])=[O:29])[CH:10]=[C:9]([F:26])[C:8]=1[N:5]1[CH2:4][CH2:3][S:2](=[O:27])(=[O:1])[CH2:7][CH2:6]1

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 962WaterHCID 9931003Pnu-288034

생성물 1

HCID 9922094Thiomorpholine, 4-(2,6-difluoro-4-nitrophenyl)-, 1,1-dioxide수율 94.2%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a suspension of the product of example 1 (300 g, 1.21 mol) in 3 L of acetic acid, nitric acid (255 mL, ca. 6 mol, fuming, 90%) is added over 30 min at room temperature. Yellow precipitate is formed within minutes and increases over time. The reaction is kept at room temperature for 18 hours, before it is poured into 6 L of water. After stirred for 2 hours, the yellow suspension is filtered. The precipitate is washed with water (1.5 L×3) and EtOH (0.5 L×2) and dried in oven at 50° C. overnight to give 333 g (94%) of the title compound as a solid.

후처리

  1. additionis added over 30 min at room temperature
  2. customYellow precipitate is formed within minutes
  3. temperatureincreases over time
  4. filtrationthe yellow suspension is filtered
  5. washThe precipitate is washed with water (1.5 L×3) and EtOH (0.5 L×2)
  6. customdried in oven at 50° C. overnight

출처 및 근거

ORD 기록
ord-005797f02363405c9b410f8b0a949391
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06605609B2

연결된 노트

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