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

HRID 267537

反応式

HRID 267537 の反応式
[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]

参加物

6

反応物 4

HCID 1049Pyridine2 回HCID 6348Carbon DisulfideHCID 11192Zinc AcetateHCID 990292-(Trichloromethyl)oxazolidine

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-62e22082b8194981b6e53d37da168fc8
出典データセット
uspto-grants-1976_03
特許番号
US03943143

関連ノート

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