Carbon Disulfide → Zinc Bis(2-trichloromethyl-3-oxazolidinecarbodithioate)

HRID 1283824

反応式

HRID 1283824 の反応式
[Cl:1][C:2]([Cl:9])([Cl:8])[CH:3]1[NH:7][CH2:6][CH2:5][O:4]1.[C:10](=[S:12])=[S:11].C([O-])(=O)C.[Zn+2:17].C([O-])(=O)C>C(O)(C)C.O>[Cl:1][C:2]([Cl:9])([Cl:8])[CH:3]1[N:7]([C:10]([S-:12])=[S:11])[CH2:6][CH2:5][O:4]1.[Cl:1][C:2]([Cl:9])([Cl:8])[CH:3]1[N:7]([C:10]([S-:12])=[S:11])[CH2:6][CH2:5][O:4]1.[Zn+2:17]

参加物

6

反応物 3

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

生成物 1

HCID 21503229Zinc Bis(2-trichloromethyl-3-oxazolidinecarbodithioate)

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3776Isopropanol溶媒

実験手順

95 2/10 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 2 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:

後処理

  1. temperatureThe reaction mixture was heated for 2 hours at 45° - 50°C
  2. filtrationthe precipitated product was filtered
  3. washwashed thoroughly with water
  4. customdried in vacuo
  5. customto give 86.3 g
  6. extractionHot benzene extractions of the crude product
  7. customgave 38 g
  8. customsintering at 208°C

出典と根拠

ORDレコード
ord-e7c69df9ef1e4be2b9d6f130b850c0fc
出典データセット
uspto-grants-1976_08
特許番号
US03976648

関連ノート

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