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Formamide → N-(1,3,4,9-tetrahydro-2H-carbazol-2-yl)formamide

HRID 66790
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HRID 66790 반응식
[CH2:1]1[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH2:4][CH2:3][CH:2]1[NH2:14].[CH:15](N)=[O:16]>O>[CH2:1]1[C:13]2[NH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH2:4][CH2:3][CH:2]1[NH:14][CH:15]=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 713FormamideHCID 205292292,3,4,9-tetrahydro-1H-carbazol-2-amine

생성물 1

HCID 20529254N-(1,3,4,9-tetrahydro-2H-carbazol-2-yl)formamide

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 8.90 g (0.048 mol) of 2,3,4,9-tetrahydro-1H-carbazol-2-amine and 65 ml of dry formamide was stirred and heated under N2 for 5 hr at 95°-100° C. The cooled reaction mixture was poured into H2O, and the precipitated gum extracted with CHCl3. The combined extracts were washed with 0.1 N HCl, 5% aqueous NaHCO3, and H2O, and dried. Et2O-trituration of the residue remaining after evaporation of the CHCl3 gave a tan solid, 8.58 g, mp 123°-126°. For analysis, it was necessary to dry the recrystallized (EtOH) sample at 120° (P2O5, 0.02 mm, 20 hr), mp 169°-171°.

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후처리

  1. temperatureheated under N2 for 5 hr at 95°-100° C
  2. customThe cooled reaction mixture
  3. extractionthe precipitated gum extracted with CHCl3
  4. washThe combined extracts were washed with 0.1 N HCl, 5% aqueous NaHCO3, and H2O
  5. customdried
  6. customafter evaporation of the CHCl3
  7. customgave a tan solid, 8.58 g, mp 123°-126°
  8. customto dry the
  9. customrecrystallized (EtOH) sample at 120° (P2O5, 0.02 mm, 20 hr), mp 169°-171°

출처 및 근거

ORD 기록
ord-a66a51a909944e09b6a14c438d190aad
출처 데이터셋
uspto-grants-1982_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04343812

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