Ammonium Acetate → 1-Methyl-2-(2,4,6-tribromo-phenoxy)-ethylamine

HRID 2189961노트

반응식

HRID 2189961 반응식
[Br:1][C:2]1[CH:12]=[C:11]([Br:13])[CH:10]=[C:9]([Br:14])[C:3]=1[O:4][CH2:5][C:6](=O)[CH3:7].C([O-])(=O)C.[NH4+].C([BH3-])#[N:21].[Na+]>CO>[CH3:7][CH:6]([NH2:21])[CH2:5][O:4][C:3]1[C:2]([Br:1])=[CH:12][C:11]([Br:13])=[CH:10][C:9]=1[Br:14]

참가 물질

5

반응물 3

HCID 517165Ammonium AcetateHCID 33030042,4,6-TribromophenoxyacetoneHCID 5003444Sodium cyanoborohydride

생성물 1

HCID 452831771-Methyl-2-(2,4,6-tribromo-phenoxy)-ethylamine수율 32%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
0 °C

실험 절차

To a solution of 1 g 1-(2,4,6-tribromo-phenoxy)-propan-2-one (2.6 mmol) in 20 ml methanol is added 2.9 g ammonium acetate (39 mmol). The mixture is cooled to 0° C. and 0.81 g sodiumcyanoborohydride (13 mmol) is added. The reaction mixture is stirred overnight at ambient temperature. The completion of the reaction is confirmed by TLC. The reaction mixture is concentrated and the remaining residue is dissolved with 1.5 N HCl and washed with diethylether. The aqueous layer is neutralised and extracted with ethylacetate. The ethylacetate layer is dried over anhydrous sodium sulphate and the solvent removed. 0.32 g 1-methyl-2-(2,4,6-tribromo-phenoxy)-ethylamine (32%) is obtained.

후처리

  1. concentrationThe reaction mixture is concentrated
  2. dissolutionthe remaining residue is dissolved with 1.5 N HCl
  3. washwashed with diethylether
  4. extractionextracted with ethylacetate
  5. dry with materialThe ethylacetate layer is dried over anhydrous sodium sulphate
  6. customthe solvent removed

출처 및 근거

ORD 기록
ord-a0968f2ae70d429b94778511187801b7
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08324263B2

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