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

HRID 1901642노트

반응식

HRID 1901642 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-8f6dddd39926469f858d4813f83b0121
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05578627

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