Hydrochloric Acid → 2-(4-Cyclopropylpiperazin-1-yl)benzothiazol-6-ylamine

HRID 1944683ノート

反応式

HRID 1944683 の反応式
[CH:1]1([N:4]2[CH2:9][CH2:8][N:7]([C:10]3[S:11][C:12]4[CH:18]=[C:17]([NH:19]C(=O)C)[CH:16]=[CH:15][C:13]=4[N:14]=3)[CH2:6][CH2:5]2)[CH2:3][CH2:2]1.Cl.[OH-].[Na+]>CCO>[CH:1]1([N:4]2[CH2:5][CH2:6][N:7]([C:10]3[S:11][C:12]4[CH:18]=[C:17]([NH2:19])[CH:16]=[CH:15][C:13]=4[N:14]=3)[CH2:8][CH2:9]2)[CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 23728857N-[2-(4-cyclopropylpiperazin-1-yl)benzothiazol-6-yl]acetamide

生成物 1

HCID 595888042-(4-Cyclopropylpiperazin-1-yl)benzothiazol-6-ylamine収率 87%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of N-[2-(4-cyclopropylpiperazin-1-yl)benzothiazol-6-yl]-acetamide (679 mg, 2.15 mmol) in EtOH (36 mL) was added concentrated hydrochloric acid (7.2 mL). The mixture was heated at reflux for 2 h. After cooling, the mixture was neutralized with 15% sodium hydroxide. The volatiles were removed under reduced pressure and the residue was dissolved in methanol (10 mL). The mixture was filtered and the filtrate was concentrated in vacuo to give 512 mg (87%) of 2-(4-cyclopropylpiperazin-1-yl)benzothiazol-6-ylamine.

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 2 h
  3. temperatureAfter cooling
  4. customThe volatiles were removed under reduced pressure
  5. dissolutionthe residue was dissolved in methanol (10 mL)
  6. filtrationThe mixture was filtered
  7. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-9d5a32afb86c40eda51abf4fa27617ce
出典データセット
uspto-grants-2013_03
特許番号
US08394842B2

反応ノート

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