Formaldehyde → 3-[(4-methylpiperazin-1-yl)methyl]-1H-indole

HRID 254189노트

반응식

HRID 254189 반응식
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[CH:3]=[CH:2]1.[CH3:10][N:11]1[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]1.[CH2:17]=O>ClCCl>[CH3:10][N:11]1[CH2:16][CH2:15][N:14]([CH2:17][C:3]2[C:4]3[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=3)[NH:1][CH:2]=2)[CH2:13][CH2:12]1

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 798IndoleHCID 531671-Methylpiperazine

생성물 1

HCID 2275843-[(4-methylpiperazin-1-yl)methyl]-1H-indole

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In a three necked round bottom flask equipped with pressure equalizing funnel, indole (1.17 g, 0.01 mole) and dichloromethane (8 mL) were taken. 1-Methylpiperazine (1.01 g, 0.011 moles) and formaldehyde (9 mL, 0.012 mole) was added slowly at room temperature and the reaction mixture was stirred well for one hour. After the completion of reaction (TLC), the product was isolated by distillation under reduced pressure. The residue was extracted with ethyl acetate (2×25 mL). The combined organic extracts were washed with water, followed by brine, dried over anhydrous sodium sulfate. The organic layer was evaporated under vacuum. The residue could either be an oily liquid or solid mass. The oily mass was triturated with n-hexane to obtain a solid material. The solid obtained was identified by IR, NMR and mass spectral analyses.

후처리

  1. customIn a three necked round bottom flask equipped with pressure
  2. customAfter the completion of reaction (TLC)
  3. customthe product was isolated by distillation under reduced pressure
  4. extractionThe residue was extracted with ethyl acetate (2×25 mL)
  5. washThe combined organic extracts were washed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe organic layer was evaporated under vacuum
  8. customThe oily mass was triturated with n-hexane
  9. customto obtain a solid material
  10. customThe solid obtained

출처 및 근거

ORD 기록
ord-f91cdf5d70774916aca3c0f30b8af2e5
출처 데이터셋
uspto-grants-2011_01
특허 번호
US07875605B2

반응 노트

불러오는 중…