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Formaldehyde → HCID 21270045, 화합물

HRID 1194347
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HRID 1194347 반응식
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]([C:11](=[O:13])[CH3:12])=[C:3]1[CH3:14].[CH2:15]=O.Cl.[CH3:18][NH:19][CH3:20]>C(O)C>[CH3:18][N:19]([CH3:15])[CH2:20][CH2:12][C:11]([C:4]1[C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[N:2]([CH3:1])[C:3]=1[CH3:14])=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 712FormaldehydeHCID 10473Dimethylamine, hydrochlorideHCID 2857551-(1,2-dimethyl-1H-indol-3-yl)ethanone

생성물 1

HCID 21270045HCID 21270045, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 1-(1,2-dimethyl-1H-indol-3-yl)-1-ethanone (0.9 g), paraformaldehyde (0.43 g) and dimethylamine hydrochloride (1.2 g) in ethanol (60 ml) was heated at reflux for 18 h, cooled, and the solvent evaporated in vacuo. The residue was partitioned between sodium carbonate (2N; 50 ml) and ethyl acetate (2×50 ml) and the combined organic extracts were dried and evaporated in vacuo to give an oil. This oil was chromatographed eluting with System A to give the title compound, which on standing gave crystals (0.9 g), m.p. 96°-98°.

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 18 h
  3. temperaturecooled
  4. customthe solvent evaporated in vacuo
  5. customThe residue was partitioned between sodium carbonate (2N; 50 ml) and ethyl acetate (2×50 ml)
  6. customthe combined organic extracts were dried
  7. customevaporated in vacuo
  8. customto give an oil
  9. customThis oil was chromatographed
  10. washeluting with System A

출처 및 근거

ORD 기록
ord-e02d5304419841458093e9e28ad2f016
출처 데이터셋
uspto-grants-1989_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04814344

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