Ammonia → 3-(Benzyloxy)-4-methoxyaniline

HRID 19988

반응식

HRID 19988 반응식
S(S([O-])=O)([O-])=O.[Na+].[Na+].[CH2:9]([O:16][C:17]1[CH:22]=[C:21]([N+:23]([O-])=O)[CH:20]=[CH:19][C:18]=1[O:26][CH3:27])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.N>CO>[CH2:9]([O:16][C:17]1[CH:22]=[C:21]([NH2:23])[CH:20]=[CH:19][C:18]=1[O:26][CH3:27])[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 24489Sodium DithioniteHCID 53140362-(Benzyloxy)-1-methoxy-4-nitrobenzene

생성물 1

HCID 125477223-(Benzyloxy)-4-methoxyaniline수율 35%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium dithionite (1.5 g) was added to a solution of 1-benzyloxy-2-methoxy-5-nitrobenzene (2.5 gm) in a mixture of methanol (20 ml)/aqueous ammonia (4 ml). After stirring for 12 hrs at room temperature, the solvent was removed under reduced pressure. The residue was partitioned between ethyl acetate (75 ml) and water (50 ml). The ethyl acetate layer was washed with water (25 ml), brine solution (25 ml), dried over anhydrous magnesium sulfate and concentrated under reduced pressure. Purification by flash chromatography over silica gel eluting with ethyl acetate/hexane (1:1) provided 0.771 g of 1-Benzyloxy-2-methoxy-5-aminobenzene (Yield=35%).

후처리

  1. customthe solvent was removed under reduced pressure
  2. customThe residue was partitioned between ethyl acetate (75 ml) and water (50 ml)
  3. washThe ethyl acetate layer was washed with water (25 ml), brine solution (25 ml)
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customPurification by flash chromatography over silica gel eluting with ethyl acetate/hexane (1:1)

출처 및 근거

ORD 기록
ord-a8453053421e4b9f80ed52c8b94597a9
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745490B2

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