Pyridine → Zinc Bis(2,2-dimethyloxazolidine-3-carbodithioate)

HRID 436287

反応式

HRID 436287 の反応式
[CH3:1][C:2]1([CH3:7])[NH:6][CH2:5][CH2:4][O:3]1.[C:8](=[S:10])=[S:9].N1C=CC=CC=1.C([O-])(=O)C.[Zn+2:21].C([O-])(=O)C>C(Cl)(Cl)Cl.C(O)C>[CH3:1][C:2]1([CH3:7])[N:6]([C:8]([S-:10])=[S:9])[CH2:5][CH2:4][O:3]1.[CH3:1][C:2]1([CH3:7])[N:6]([C:8]([S-:10])=[S:9])[CH2:5][CH2:4][O:3]1.[Zn+2:21]

参加物

7

反応物 4

HCID 1049PyridineHCID 6348Carbon DisulfideHCID 11192Zinc AcetateHCID 5506972,2-Dimethyl-oxazolidine

生成物 1

HCID 21453996Zinc Bis(2,2-dimethyloxazolidine-3-carbodithioate)

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 6212Chloroform溶媒

実験手順

While cooling and stirring, 20 g. (0.20 mole) of 2,2-dimethyloxazolidine (preparation described by E. Bergmann et. al., J. Am. Chem. Soc. 75, 358 (1953)) was added to a solution of 15.2 g. (0.20 mole) carbon disulfide in 150 g. pyridine. To the stirring solution was added 18.3 g. (0.10 mole) of anhydrous zinc acetate at 25°-30° C. After standing overnight at room temperature, filtration gave 15.2 g. of the crude product; vacuum-concentration of the filtrate and ethanol-dilution of the residue gave an additional 10.4 g. After combining and vacuum-drying of the crude product at 100° C there was obtained 17.8 g. of the desired carbodithioate melting at 188°- 190° C (decomp.). A small sample, dissolved in hot chloroform and precipitated by hexane (m. 192°-3° C decomp.) had the following analysis: Found: C, 34.22; H, 4.47; N, 6.84; Zn, 15.20%. Calcd for C12H20N2O2S4Zn: C, 34.50; H, 4.79; N, 6.71; Zn, 15.67%.

後処理

  1. temperatureWhile cooling
  2. additionTo the stirring solution was added 18.3 g
  3. customat 25°-30° C
  4. filtrationfiltration
  5. customgave 15.2 g
  6. dry with materialvacuum-drying of the crude product at 100° C
  7. customthere was obtained 17.8 g
  8. customprecipitated by hexane (m. 192°-3° C decomp.)

出典と根拠

ORDレコード
ord-2a01b3882ec84cc6ae7beccbd576ba85
出典データセット
uspto-grants-1977_02
特許番号
US04008244

関連ノート

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