Hydrochloric Acid → 3-[2-Amino-3-(4-imidazolyl)propoxy]-5-chloro-1,2-benzoisoxazole dihydrochloride

HRID 1901642ノート

反応式

HRID 1901642 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7]([O:10][CH2:11][CH:12]([NH:38]C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[CH2:13][C:14]3[N:15]=[CH:16][N:17](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[CH:18]=3)[C:6]=2[CH:58]=1.CC(O)C.[ClH:63]>C(Cl)Cl>[ClH:1].[ClH:63].[NH2:38][CH:12]([CH2:13][C:14]1[N:15]=[CH:16][NH:17][CH:18]=1)[CH2:11][O:10][C:7]1[C:6]2[CH:58]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[O:9][N:8]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 233683685-Chloro-3-[2-tritylamino-3-(1-trityl-4-imidazolyl)propoxy]-1,2-benzoisoxazole

生成物 1

HCID 1784787063-[2-Amino-3-(4-imidazolyl)propoxy]-5-chloro-1,2-benzoisoxazole dihydrochloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 0.91 g of 5-chloro-3-[2-tritylamino-3-(1-trityl-4-imidazolyl)propoxy]-1,2-benzoisoxazole in 2 ml of methylene chloride is added 2.2 ml of a 2-propanol solution (6.5M) of hydrogen chloride at room temperature, and they are subjected to reaction at the same temperature for 24 hours, after which the solvent is removed by distillation under reduced pressure. Diisopropyl ether is added to the residue obtained and the crystals precipitated are collected by filtration, to obtain 0.4 g of colorless, crystalline 3-[2-amino-3-(4-imidazolyl)propoxy]-5-chloro-1,2-benzoisoxazole dihydrochloride having a melting point of 246.0°-248.4° C. (decomp.).

後処理

  1. customthey are subjected to reaction at the same temperature for 24 hours
  2. customafter which the solvent is removed by distillation under reduced pressure
  3. additionDiisopropyl ether is added to the residue
  4. customobtained
  5. customthe crystals precipitated
  6. filtrationare collected by filtration

出典と根拠

ORDレコード
ord-8f6dddd39926469f858d4813f83b0121
出典データセット
uspto-grants-1996_11
特許番号
US05578627

反応ノート

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