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

HRID 1901656ノート

反応式

HRID 1901656 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:19]C(OC(C)(C)C)=O)[CH2:13][O:14][C:15](=[S:18])[NH:16][CH3:17])[C:6]=2[CH:27]=1.O1CCOCC1.Cl.CC(O)C>CO>[ClH:1].[NH2:19][CH:12]([CH2:13][O:14][C:15](=[S:18])[NH:16][CH3:17])[CH2:11][O:10][C:7]1[C:6]2[CH:27]=[C:2]([Cl:1])[CH:3]=[CH:4][C:5]=2[O:9][N:8]=1

参加物

6

実験手順

To a solution of 0.4 g of 5-chloro-3-(2-tert-butoxycarbonylamino-3-methylthiocarbamoyloxypropoxy)-1,2-benzoisoxazole in 10 ml of methanol is added 5 ml of a dioxane solution (3.2N) of hydrogen chloride at room temperature, and they are subjected to reaction at the same temperature for three hours, after which the solvent is removed by distillation under reduced pressure. To the residue obtained is added 3 ml of 2-propanol, and the crystals precipitated are collected by filtration, to obtain 0.22 g of pale yellow, crystalline 3-(2-amino-3-methylthiocarbamoyloxypropoxy)-5-chloro-1,2-benzoisoxazole hydrochloride having a melting point of 198.8°-199.2° C. (decomp.).

後処理

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

出典と根拠

ORDレコード
ord-f79c01ee8c7d48ef8f1fc8bdf01e255d
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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