Sodium Hydroxide → 2-Amino-3-chloro-7-ethyl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine hydrochloride

HRID 1153767ノート

反応式

HRID 1153767 の反応式
[NH2:1][C:2]1[CH:3]=[N:4][C:5]2[CH2:11][CH2:10][N:9]([CH2:12][CH3:13])[CH2:8][CH2:7][C:6]=2[N:14]=1.[Cl:15]Cl.[OH-].[Na+]>C(O)(=O)C>[ClH:15].[NH2:1][C:2]1[C:3]([Cl:15])=[N:4][C:5]2[CH2:11][CH2:10][N:9]([CH2:12][CH3:13])[CH2:8][CH2:7][C:6]=2[N:14]=1

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 24526ChlorineHCID 30678372-Amino-7-ethyl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine

生成物 1

HCID 204363752-Amino-3-chloro-7-ethyl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine hydrochloride

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

6 gm (31.3 mmols) of 2-amino-7-ethyl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine were dissolved in 100 ml of glacial acetic acid and, while cooling the solution with ice, chlorine was introduced until the thin-layer chromatogram showed that no more starting material was present. Thereafter, the reaction mixture was made alkaline with 2N sodium hydroxide and was then extracted with chloroform. The chloroform extract solution was evaporated, and the residue was column-chromatographically purified on silicagel with ethyl acetate/methanol/ethanolic ammonia (4:1:0.5) as the mobile phase. The hydrochloride was precipitated from ethanol with ethanolic hydrochloric acid.

後処理

  1. additionwas introduced until the thin-layer chromatogram
  2. extractionwas then extracted with chloroform
  3. extractionThe chloroform extract solution
  4. customwas evaporated
  5. custompurified on silicagel with ethyl acetate/methanol/ethanolic ammonia (4:1:0.5) as the mobile phase
  6. customThe hydrochloride was precipitated from ethanol with ethanolic hydrochloric acid

出典と根拠

ORDレコード
ord-9b0741da2cc849b5a41a35cee172d755
出典データセット
uspto-grants-1984_12
特許番号
US04486433

反応ノート

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