関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Carbon Disulfide | HCID 6348 | — |
| 反応物 | Zinc Acetate | HCID 11192 | — |
| 反応物 | 2-(Trichloromethyl)oxazolidine | HCID 99029 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | Zinc Bis(2-trichloromethyl-3-oxazolidinecarbodithioate) | HCID 21503229 | — |
反応手順
Ninety-five and two-tenths g. of 2-trichloromethyloxazolidine (preparation described by W. Ruske and I. Hartmann J. Prakt, Chem. 18 146 (1962) was dissolved in a mixture of 300 ml isopropanol, and 50.5 g. (0.50 mole) of carbon disulfide was added dropwise followed by 43.9 g. (0.25 mole) of anhydrous zinc acetate. The reaction mixture was heated for two hours at 45°- 50°C, cooled to room temperature, and diluted with 1 liter water; the precipitated product was filtered, washed thoroughly with water and dried in vacuo to give 86.3 g. of the crude product, melting at 193°-195°C (decomp.). Hot benzene extractions of the crude product gave 38 g. of the desired carbodithioate sintering at 208°C, and melting 213°- 216°C (decomp.). It had the following analysis: Found: C, 20.19; H, 2.08; N, 4.67; S, 20.96%. Calcd for C10H10Cl6N2O2S4Zn: C, 20.12; H, 1,68; N, 4.69; S, 21.46%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US03943143 |
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| 出典データセット | uspto-grants-1976_03 |
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| ORD ID | ord-0b5588cc1397498f83775e4a0d984fa8 |
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| 出典メモ | uspto-grants-1976_03 |
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