Formaldehyde → Benzyl(methoxymethyl)((trimethylsilyl)methyl)amine

HRID 504391

반응식

HRID 504391 반응식
[CH2:1]=O.[CH2:3]([NH:10][CH2:11][Si:12]([CH3:15])([CH3:14])[CH3:13])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.CO.[C:18](=[O:21])([O-])[O-].[K+].[K+]>CCOCC>[CH2:3]([N:10]([CH2:1][O:21][CH3:18])[CH2:11][Si:12]([CH3:15])([CH3:14])[CH3:13])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

참가 물질

6

반응물 4

HCID 712FormaldehydeHCID 887MethanolHCID 11430Potassium Carbonate2회HCID 353458N-[(Trimethylsilyl)methyl]benzylamine

생성물 1

HCID 353442Benzyl(methoxymethyl)((trimethylsilyl)methyl)amine

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
0 °C

실험 절차

Into a round bottom 3-neck flask equipped with a nitrogen flow and a magnetic stirrer was added formaldehyde (74.000 mmol, 7.4000×10−2 mol) (as a 37% aqueous solution). The flask was cooled to 0° C. and N-benzyl-N-(trimethylsilyl)methylamine (10.000 g, 5.1716790×10−2 mol) was added dropwise with stirring. After stirring for 10 minutes at 0° C., methanol (6.000 mL, 0.14811874 mol) was added in one portion. Potassium carbonate (4.000 g, 2.8942408×10−2 mol) was added to the mixture to absorb the aqueous phase. The mixture was stirred for one hour, then the nonaqueous phase decanted, and then potassium carbonate (2.000 g, 1.4471204×10−2 mol) was added. The mixture was stirred at 25° C. for 12 hours. Ether is added to the mixture and the solution was dried over potassium carbonate, filtered and concentrated under reduced pressure. The residue is distilled at reduced pressure to give the product as a colorless liquid.

후처리

  1. customInto a round bottom 3-neck flask equipped with a nitrogen flow and a magnetic stirrer
  2. stirringAfter stirring for 10 minutes at 0° C.
  3. customto absorb the aqueous phase
  4. stirringThe mixture was stirred for one hour
  5. customthe nonaqueous phase decanted
  6. stirringThe mixture was stirred at 25° C. for 12 hours
  7. dry with materialthe solution was dried over potassium carbonate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure
  10. distillationThe residue is distilled at reduced pressure

출처 및 근거

ORD 기록
ord-b67d6de4eff343b4a4a87926200b9ed2
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07776874B2

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