4-(4-Nitrophenyl)thiomorpholine 1,1-dioxide → 4-(4-Aminophenyl)thiomorpholine 1,1-Dioxide

HRID 1910821노트

반응식

HRID 1910821 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([N:10]2[CH2:15][CH2:14][S:13](=[O:17])(=[O:16])[CH2:12][CH2:11]2)=[CH:6][CH:5]=1)([O-])=O>C(O)(=O)C.[Zn]>[O:17]=[S:13]1(=[O:16])[CH2:12][CH2:11][N:10]([C:7]2[CH:6]=[CH:5][C:4]([NH2:1])=[CH:9][CH:8]=2)[CH2:15][CH2:14]1

참가 물질

4

반응물 1

HCID 114595184-(4-Nitrophenyl)thiomorpholine 1,1-dioxide

생성물 1

HCID 263703844-(4-Aminophenyl)thiomorpholine 1,1-Dioxide수율 51.6%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

반응 조건

온도
60 °C

실험 절차

Zinc powder (0.47 g, 7.2 mmol) was added to a solution of 4-(4-nitro-phenyl)-thiomorpholine 1,1-dioxide (155 mg, 0.60 mmol) in acetic acid (3 mL) and the mixture was stirred at 60° C. for 2 h. The reaction mixture was concentrated to dryness, diluted with ethyl acetate and washed with sodium bicarbonate solution and water then dried over sodium sulfate. The organic layer was concentrated to dryness to afford 4-(1,1-dioxo-1λ6-thiomorpholin-4-yl)-phenylamine (70 mg, 51%).

후처리

  1. concentrationThe reaction mixture was concentrated to dryness
  2. additiondiluted with ethyl acetate
  3. washwashed with sodium bicarbonate solution and water
  4. dry with materialthen dried over sodium sulfate
  5. concentrationThe organic layer was concentrated to dryness

출처 및 근거

ORD 기록
ord-175e5fda9a604c0e9908885033786874
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08604029B2

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