Methanol → N-(3-Amino-4-chlorophenyl)-3,4,5,6-tetrahydrophthalimide

HRID 1903894노트

반응식

HRID 1903894 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([N:11]2[C:15](=[O:16])[C:14]3[CH2:17][CH2:18][CH2:19][CH2:20][C:13]=3[C:12]2=[O:21])[CH:7]=[CH:8][C:9]=1[Cl:10])([O-])=O.CO>O=[Pt]=O.CCOC(C)=O>[NH2:1][C:4]1[CH:5]=[C:6]([N:11]2[C:15](=[O:16])[C:14]3[CH2:17][CH2:18][CH2:19][CH2:20][C:13]=3[C:12]2=[O:21])[CH:7]=[CH:8][C:9]=1[Cl:10]

참가 물질

5

반응물 2

HCID 887MethanolHCID 1568791H-Isoindole-1,3(2H)-dione, 2-(4-chloro-3-nitrophenyl)-4,5,6,7-tetrahydro-

생성물 1

HCID 13285967N-(3-Amino-4-chlorophenyl)-3,4,5,6-tetrahydrophthalimide수율 80.4%

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 40 g of N-(3-nitro-4-chlorophenyl)-3,4,5,6-tetrahydrophthalimide in 900 ml. of MeOH and 100 ml. of EtOAc in a hydrogenation bottle is added 0.5 g PtO2. The bottle is purged with hydrogen then pressurized to 50 psig and shaken until the required amount of H2 was used. The reaction mixture was filtered through celite, washed well with CH2Cl2 and the combined organic phases concentrated in vacuo to yield 29 g of the product. This product was used without further purification in subsequent transformations.

후처리

  1. customThe bottle is purged with hydrogen
  2. filtrationThe reaction mixture was filtered through celite
  3. washwashed well with CH2Cl2
  4. concentrationthe combined organic phases concentrated in vacuo

출처 및 근거

ORD 기록
ord-6274814401c3424bb806403038c81f40
출처 데이터셋
uspto-grants-1984_03
특허 번호
US04439229

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