Hydrochloric Acid → 5-Chloro-3-[2-(2-methyl-1,3-thiazol-5-yl)-2-aminoethoxy]-1,2-benzoisoxazole hydrochloride

HRID 1901629ノート

反応式

HRID 1901629 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]([C:33]3[S:37][C:36]([CH3:38])=[N:35][CH:34]=3)[NH:13]C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)[C:6]=2[CH:39]=1.CC(O)C.Cl>C(Cl)(Cl)Cl.CO>[ClH:1].[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[O:9][N:8]=[C:7]([O:10][CH2:11][CH:12]([C:33]3[S:37][C:36]([CH3:38])=[N:35][CH:34]=3)[NH2:13])[C:6]=2[CH:39]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 3776Isopropanol2 回HCID 233685165-Chloro-3-[2-(2-methyl-1,3-thiazol-5-yl)-2-tritylaminoethoxy]-1,2-benzoisoxazole

生成物 1

HCID 233685375-Chloro-3-[2-(2-methyl-1,3-thiazol-5-yl)-2-aminoethoxy]-1,2-benzoisoxazole hydrochloride

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6212Chloroform溶媒

実験手順

To a solution of 1.7 g of 5-chloro-3-[2-(2-methyl-1,3-thiazol-5-yl)-2-tritylaminoethoxy]-1,2-benzoisoxazole in 17 ml of chloroform and 17 ml of methanol is added 2.05 ml of a 2-propanol solution (7.5N) of hydrogen chloride at room temperature, and they are subjected to reaction at the same temperature for two hours, after which the solvent is removed by distillation under reduced pressure. To the residue obtained is added 2-propanol, and after stirring, the crystals precipitated are collected by filtration, to obtain 0.90 g of colorless, crystalline 5-chloro-3-[2-(2-methyl-1,3-thiazol-5-yl)-2-aminoethoxy]-1,2-benzoisoxazole hydrochloride having a melting point of 212° C.

後処理

  1. customthey are subjected to reaction at the same temperature for two 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-718cfeffa83a4723b3c85a6fc47989c7
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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