Pyridine → Zinc Bis (2-trichloromethyl-3-oxazolidinecarbodithioate) Pyridine

HRID 267537

반응식

HRID 267537 반응식
[Cl:1][C:2]([Cl:9])([Cl:8])[CH:3]1[NH:7][CH2:6][CH2:5][O:4]1.[N:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[C:16](=[S:18])=[S:17].C([O-])(=O)C.[Zn+2:23].C([O-])(=O)C>O>[N:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.[Cl:1][C:2]([Cl:9])([Cl:8])[CH:3]1[N:7]([C:16]([S-:18])=[S:17])[CH2:6][CH2:5][O:4]1.[Cl:1][C:2]([Cl:9])([Cl:8])[CH:3]1[N:7]([C:16]([S-:18])=[S:17])[CH2:6][CH2:5][O:4]1.[Zn+2:23]

참가 물질

6

반응물 4

HCID 1049Pyridine2회HCID 6348Carbon DisulfideHCID 11192Zinc AcetateHCID 990292-(Trichloromethyl)oxazolidine

생성물 1

HCID 86733117Zinc Bis (2-trichloromethyl-3-oxazolidinecarbodithioate) Pyridine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Thirty and four-tenth grams (0.160 mole) of 2-trichloromethyloxazolidine (preparation described by W. Ruske and I. Hartmann, J. Prakt. Chem. 18, 146 (1962) was dissolved in 480 g. of pyridine. With rapid stirring at room temperature, 14.4 g. (0.184 mole) of carbon disulfide was added dropwise followed by 15.2 g. (0.083 mole) of anhydrous zinc acetate. The reaction mixture was heated 3 hours at 45°- 50°C, cooled to room temperature, and then diluted with 1 liter water; the precipitated product was filtered and dried in vacuo at room temperature to obtain 33.4 g. of the desired pyridine adduct melting at 205°- 207°C (decomp.). A small analytical sample, recrystallized in methanol, sintered at 209°C and melted with decomposition at 212°-214°C. It had the following anaylsis: Found: C, 26.70; H, 2.74; N, 6.30; S, 19.60; Cl, 31.37; Zn, 9.55%. Calcd for C10H10Cl6N2O2S4Zn . C5H5N: C, 26.65; H, 2.22; N, 6.23; S, 18.95 Cl, 31.54; Zn, 9.68%.

후처리

  1. dissolution18, 146 (1962) was dissolved in 480 g
  2. temperatureThe reaction mixture was heated 3 hours at 45°- 50°C
  3. temperaturecooled to room temperature
  4. filtrationthe precipitated product was filtered
  5. customdried in vacuo at room temperature
  6. customto obtain 33.4 g
  7. customA small analytical sample, recrystallized in methanol
  8. customsintered at 209°C
  9. custommelted with decomposition at 212°-214°C

출처 및 근거

ORD 기록
ord-62e22082b8194981b6e53d37da168fc8
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03943143

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