Hydrochloric Acid → 3-(2-Amino-3-cyanopropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride

HRID 1901647노트

반응식

HRID 1901647 반응식
C(OC([NH:8][CH:9]([CH2:22][C:23]#[N:24])[CH2:10][O:11][C:12]1[C:16]2[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=2[O:14][N:13]=1)=O)(C)(C)C.CC(O)C.Cl.C(OC(C)C)(C)C>CO>[ClH:21].[NH2:8][CH:9]([CH2:22][C:23]#[N:24])[CH2:10][O:11][C:12]1[C:16]2[CH:17]=[C:18]([Cl:21])[CH:19]=[CH:20][C:15]=2[O:14][N:13]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 3776IsopropanolHCID 7914Diisopropyl EtherHCID 233685283-(2-Tert-butoxycarbonylamino-3-cyanopropoxy)-5-chloro-1,2-benzoisoxazole

생성물 1

HCID 233684313-(2-Amino-3-cyanopropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a suspension of 1.0 g of 3-(2-tert-butoxycarbonylamino-3-cyanopropoxy)-5-chloro-1,2-benzoisoxazole in 15 ml of methanol is added 7.8 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 seven hours. Thereafter, the solvent is removed by distillation under reduced pressure. To the residue obtained is added diisopropyl ether, and the crystals precipitated are collected by filtration, to obtain 0.78 g of colorless, crystalline 3-(2-amino-3-cyanopropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride having a melting point of 188.8°-190.9° C. (decomp.).

후처리

  1. customthey are subjected to reaction at the same temperature for seven hours
  2. customThereafter, the solvent is removed by distillation under reduced pressure
  3. customTo the residue obtained
  4. customthe crystals precipitated
  5. filtrationare collected by filtration

출처 및 근거

ORD 기록
ord-1c4d6d544f1e4798b912a69b9d8488f1
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05578627

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