Carbon Disulfide → HCID 178504226, 화합물

HRID 1890951노트

반응식

HRID 1890951 반응식
[CH3:1][Si:2]([CH3:21])([CH3:20])[CH2:3][CH2:4][O:5][CH2:6][N:7]1[CH:11]=[C:10]([C:12]2[N:17]=[N:16][C:15]([NH:18][NH2:19])=[CH:14][CH:13]=2)[CH:9]=[N:8]1.C([O-])([O-])=O.[K+].[K+].[C:28](=S)=[S:29]>C(O)C.O>[CH3:1][Si:2]([CH3:21])([CH3:20])[CH2:3][CH2:4][O:5][CH2:6][N:7]1[CH:11]=[C:10]([C:12]2[CH:13]=[CH:14][C:15]3[N:16]([C:28]([SH:29])=[N:19][N:18]=3)[N:17]=2)[CH:9]=[N:8]1

참가 물질

6

반응물 3

HCID 6348Carbon DisulfideHCID 11430Potassium CarbonateHCID 68975416{6-[1-(2-Trimethylsilanyl-ethoxymethyl)-1H-pyrazol-4-yl]-pyridazin-3-yl}-hydrazine

생성물 1

HCID 178504226HCID 178504226, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

To a solution of {6-[1-(2-trimethylsilanyl-ethoxymethyl)-1H-pyrazol-4-yl]-pyridazin-3-yl}-hydrazine (490 mg, 1.6 mmol) in ethanol (6.5 mL) and water (1.8 mL) was added K2CO3 (359 mg, 2.6 mmol), followed by CS2 (0.212 mL, 3.5 mmol). The mixture was stirred and heated at 80° C. for 3 h under nitrogen atmosphere. The mixture was cooled to room temperature and concentrated to 50% volume in vacuo and acidified to pH 1 with 1 N aqueous HCl. The resulting precipitate was collected, washed with water, and dried in vacuo to provide title compound as a dark red solid (quantitative yield): 1H NMR (DMSO-d6) δ 0.01 (9H, s), 0.90 (2H, t), 3.63 (2H, t), 5.56 (2H, s), 7.82 (1H, d), 8.24 (1H, d), 8.27 (1H, s), 8.80 (1H, s), 15.23 (1H, bs); MS (m/z) 349 [M+H]+.

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. concentrationconcentrated to 50% volume in vacuo
  3. customThe resulting precipitate was collected
  4. washwashed with water
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-1bef38ff57354014950cc9e49ea2df5f
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507489B2

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