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

HRID 402737노트

반응식

HRID 402737 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매2회HCID 8857Ethyl Acetate용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-4da62a82c56d468a8489f3d58f90a5de
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08742113B2

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