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Hydrogen Sulfide → HCID 12278977, 화합물

HRID 442137
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HRID 442137 반응식
[C:1]1([C:7]2[CH:16]=[CH:15][C:14]3[CH2:13][CH2:12][CH2:11][CH:10]([C:17]#[N:18])[C:9]=3[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)CC)C.[SH2:26]>N1C=CC=CC=1>[C:1]1([C:7]2[CH:16]=[CH:15][C:14]3[CH2:13][CH2:12][CH2:11][CH:10]([C:17](=[S:26])[NH2:18])[C:9]=3[N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
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참가 물질

5

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HCID 402Hydrogen SulfideHCID 8471TriethylamineHCID 122789758-Quinolinecarbonitrile, 5,6,7,8-tetrahydro-2-phenyl-

생성물 1

HCID 12278977HCID 12278977, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

2-Phenyl-8-cyano-5,6,7,8-tetrahydroquinoline (2 g.) was dissolved in pyridine (5 ml.) and triethylamine (1.3 ml.) and the solution treated with H2S gas for 6 hours and the reaction mixture allowed to stand at room temperature for 12 hours. The solvent was removed and the residual oil dissolved in dilute HCl, extracted with ether (2 × 50 ml.) and the extracts discarded. The aqueous solution was made basic and extracted into chloroform (3 × 50 ml.). The combined extracts were dried and evaporated in vacuo to give 2-phenyl-5,6,-7,8-tetrahydroquinoline-8-thiocarboxamide which was dissolved in ethanol (5 ml.), diluted with ether (25 ml.) and the solution saturated with HCl gas. The solvent was removed in vacuo and the residual solid recrystallised from methanol-ether giving hydrochloride of the title compound as colourless needles mpt. 211° C. Found: C, 63.41; H, 5.70; N, 8.94%. C16H16N2S. HCl requires: C, 63.04; H, 5.62; N, 9.19 %.

후처리

  1. customThe solvent was removed
  2. dissolutionthe residual oil dissolved in dilute HCl
  3. extractionextracted with ether (2 × 50 ml.)
  4. extractionextracted into chloroform (3 × 50 ml.)
  5. customThe combined extracts were dried
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-69143ca7f227472c85187db3cbd17960
출처 데이터셋
uspto-grants-1977_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04044138

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