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1,4-Dihydro-2,6-dimethyl-4-(3-isothiocyanatophenyl)-3,5-pyrazinedicarboxylic acid, dimethyl ester → HCID 178498419, 화합물

HRID 566904
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HRID 566904 반응식
[CH3:1][C:2]1[NH:3][C:4]([CH3:25])=[C:5]([C:21]([O:23][CH3:24])=[O:22])[N:6]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([N:18]=[C:19]=S)[CH:13]=2)[C:7]=1[C:8]([O:10][CH3:11])=[O:9].[N:26]#[C:27][NH2:28].[Na].[C:30]1([CH:36]2[CH2:41][CH2:40][N:39]([CH2:42][CH2:43][CH2:44][NH2:45])[CH2:38][CH2:37]2)[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1>CCO.C1COCC1.Cl[Hg]Cl>[C:27]([N:28]=[C:19]([NH:18][C:14]1[CH:13]=[C:12]([N:6]2[C:7]([C:8]([O:10][CH3:11])=[O:9])=[C:2]([CH3:1])[NH:3][C:4]([CH3:25])=[C:5]2[C:21]([O:23][CH3:24])=[O:22])[CH:17]=[CH:16][CH:15]=1)[NH:45][CH2:44][CH2:43][CH2:42][N:39]1[CH2:38][CH2:37][CH:36]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH2:41][CH2:40]1)#[N:26]
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참가 물질

7

반응물 3

HCID 155242381,4-Dihydro-2,6-dimethyl-4-(3-isothiocyanatophenyl)-3,5-pyrazinedicarboxylic acid, dimethyl esterHCID 22725156HCID 22725156, 화합물HCID 57375518Cyanamidnatrium

생성물 1

HCID 178498419HCID 178498419, 화합물

시약·촉매·용매 3

HCID 24085Mercuric Chloride촉매
HCID 702
Ethanol
용매
HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

1,4-Dihydro-2,6-dimethyl-4-(3-isothiocyanatophenyl)-3,5-pyrazinedicarboxylic acid, dimethyl ester (144 mg, 0.40 mmol) was added into sodium cyanamide (28 mg, 0.44 mmol) in 3 mL of EtOH and the mixture was stirred for 20 minutes. EtOH was then removed in vacuo and the resultant foam-like material was mixed with 4-phenyl-piperidine-1-propanamine (105 mg, 0.48 mmol) in 5 mL of THF. The mixture was cooled down to 0° C. and HgCl2 (109 mg) was added. The reaction was completed in 15 min. After filtration and extraction, the organic layer was concentrated and purified by chromatography (silica gel, eluted with 10% (v/v) methanol in methylene chloride) to yield the title compound as isolated as a yellow foam (175 mg, 75%); 1H-NMR (CDCl3) δ 7.05-7.35 (m, 6H), 6.75 (br, 1H), 6.65 (d, 1H, J=7.5 Hz), 6.58 (d, 1H, J=8.3 Hz), 6.53 (br, 1H), 5.98 (br, 1H), 3.72 (s, 6H), 3.38 (m, 2H), 2.97 (m, 2H), 2.30-2.55 (m, 3H), 2.39 (s, 6H), 2.03 (m, 2H), 1.65-1.80 (m, 4H), 1.40-1.60 (m, 2H); 13C-NMR (CDCl3) δ 166.2, 152.6, 149.4, 129.9, 128.5, 126.9, 126.3, 118.3, 116.3, 112.5, 110.4, 108.7, 54.1, 51.8, 42.4, 41.0, 32.7, 29.8, 25.6, and 17.9.

후처리

  1. customEtOH was then removed in vacuo
  2. waitThe reaction was completed in 15 min
  3. filtrationAfter filtration and extraction
  4. concentrationthe organic layer was concentrated
  5. custompurified by chromatography (silica gel, eluted with 10% (v/v) methanol in methylene chloride)

출처 및 근거

ORD 기록
ord-cb6c1ecab6774aa2844db12bb35b7db2
출처 데이터셋
uspto-grants-2001_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06177429B1

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