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

HRID 1901647ノート

反応式

HRID 1901647 の反応式
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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-1c4d6d544f1e4798b912a69b9d8488f1
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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