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

HRID 1901612ノート

反応式

HRID 1901612 の反応式
CC(O)C.Cl.C(OC([NH:13][CH:14]([CH2:27][O:28][C:29]([NH:31][CH3:32])=[O:30])[CH2:15][O:16][C:17]1[C:21]2[CH:22]=[C:23]([Cl:26])[CH:24]=[CH:25][C:20]=2[O:19][N:18]=1)=O)(C)(C)C>CO>[ClH:26].[NH2:13][CH:14]([CH2:27][O:28][C:29]([NH:31][CH3:32])=[O:30])[CH2:15][O:16][C:17]1[C:21]2[CH:22]=[C:23]([Cl:26])[CH:24]=[CH:25][C:20]=2[O:19][N:18]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 3776Isopropanol2 回HCID 23368486HCID 23368486、化合物

生成物 1

HCID 233684343-(2-Amino-3-methylaminocarbonyloxypropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In 10 ml of methanol is dissolved 3-(2-tert-butoxycarbonylamino-3-methylaminocarbonyloxypropoxy)-5-chloro-1,2-benzoisoxazole, and to this solution is added 9.6 ml of a 2-propanol solution (7.5N) of hydrogen chloride, and they are subjected to reaction at 20°-25° C. for 4.5 hours. The solvent is removed from the reaction mixture by distillation under reduced pressure, and to the residue obtained is added 5 ml of 2-propanol, after which the crystals precipitated are collected by filtration, to obtain 0.30 g of colorless, crystalline 3-(2-amino-3-methylaminocarbonyloxypropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride having a melting point of 206°-209° C.

後処理

  1. customare subjected to reaction at 20°-25° C. for 4.5 hours
  2. customThe solvent is removed from the reaction mixture by distillation under reduced pressure
  3. customto the residue obtained
  4. customafter which the crystals precipitated
  5. filtrationare collected by filtration

出典と根拠

ORDレコード
ord-303b994a51634e5d92f9986586fbfa76
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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