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

HRID 647487ノート

反応式

HRID 647487 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 2 N 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-73f2dcac85ab427baa972df7aaeca814
出典データセット
uspto-grants-1983_10
特許番号
US04409220

反応ノート

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