Acetic Acid → 1-Nitroso-4-(2,2,2-trifluoroethyl)piperazine

HRID 402737ノート

反応式

HRID 402737 の反応式
[F:1][C:2]([F:11])([F:10])[CH2:3][N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.[N:12]([O-])=[O:13].[Na+].C(O)(=O)C.C(=O)([O-])[O-].[Na+].[Na+]>O.C(OCC)(=O)C>[N:12]([N:7]1[CH2:6][CH2:5][N:4]([CH2:3][C:2]([F:1])([F:10])[F:11])[CH2:9][CH2:8]1)=[O:13]

参加物

7

反応物 4

HCID 176Acetic AcidHCID 10340Sodium CarbonateHCID 95339211-(2,2,2-Trifluoroethyl)piperazineHCID 23668193Sodium Nitrite

生成物 1

HCID 867084131-Nitroso-4-(2,2,2-trifluoroethyl)piperazine

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 1-(2,2,2-trifluoroethyl)piperazine (4.88 g, 29.0 mmol) in water (4.9 mL) that cooled with ice bath, a solution of sodium nitrite (4.04 g, 58.6 mmol) in water (20 mL) and acetic acid (5.0 mL, 87.0 mmol) were added dropwise slowly, then the mixture was stirred for 1 h. The reaction mixture was all owed to warm to ambient temperature, stirred for further 2 h. The reaction mixture was adjusted to pH9 using sodium carbonate, diluted with ethyl acetate and washed with water and brine. The organic layer was dried over magnesium sulfate and concentrated to afford 1-nitroso-4-(2,2,2-trifluoroethyl)piperazine as oil (5.57 g, y. 97%).

後処理

  1. stirringstirred for further 2 h
  2. washwashed with water and brine
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-4da62a82c56d468a8489f3d58f90a5de
出典データセット
uspto-grants-2014_06
特許番号
US08742113B2

反応ノート

読み込み中…