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Carbon Disulfide → HCID 21454007、化合物

HRID 436289
ノート
印刷プレビュー

反応式

HRID 436289 の反応式
Cl.[CH3:2][C:3]1([CH3:8])[NH:7][CH2:6][CH2:5][S:4]1.C(N(CC)CC)C.[C:16](=[S:18])=[S:17].C([O-])(=O)C.[Zn+2:23].C([O-])(=O)C>C(O)(C)C>[CH3:2][C:3]1([CH3:8])[N:7]([C:16]([S-:18])=[S:17])[CH2:6][CH2:5][S:4]1.[CH3:2][C:3]1([CH3:8])[N:7]([C:16]([S-:18])=[S:17])[CH2:6][CH2:5][S:4]1.[Zn+2:23]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6348Carbon DisulfideHCID 8471TriethylamineHCID 11192Zinc AcetateHCID 1203862,2-Dimethyl-1,3-thiazolidine--hydrogen chloride (1/1)

生成物 1

HCID 21454007HCID 21454007、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

反応条件

温度
10 °C

実験手順

While cooling and stirring at 10° C, 76.8 g. (0.50 mole) 2,2-dimethylthiazolidine hydrochloride [preparation described by B. Sweetman et al. J. Med. Chem. 12, 888 (1969)] was added to a mixture of 30 ml isopropanol and 101 g. (1.00 mole) triethylamine. Likewise, 38.0 g. (0.50 mole) of carbon disulfide was gradually added, followed by 45.8 g. (0.25 mole) of anhydrous zinc acetate. After standing ovenight at room temperature, the precipitate was filtered, twice water-washed with 1 liter portions of water and air-dried to give 80.5 g. of the yellow product melting at 148° - 153° C (decomp.) and having the following analysis: Found: C, 31.51; H, 4.70%. Calcd for C12H20N2S6Zn: C, 32.04; H, 4.45%.

後処理

  1. temperatureWhile cooling
  2. customAfter standing ovenight at room temperature
  3. filtrationthe precipitate was filtered
  4. washtwice water-washed with 1 liter portions of water
  5. customair-dried
  6. customto give 80.5 g

出典と根拠

ORDレコード
ord-46cd78d527ee4463aa74dbb2369a644b
出典データセット
uspto-grants-1977_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04008244

反応ノート

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