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

HRID 1903894ノート

反応式

HRID 1903894 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6274814401c3424bb806403038c81f40
出典データセット
uspto-grants-1984_03
特許番号
US04439229

反応ノート

読み込み中…