Sodium Hydroxide → HCID 178479362、化合物

HRID 1073817ノート

反応式

HRID 1073817 の反応式
[S:1]1[CH2:5][C:4](=[S:6])[NH:3][C:2]1=[S:7].[OH-].[Na+].Cl.[Cl:11][CH2:12][C:13]([NH2:15])=[NH:14]>C(O)C>[ClH:11].[C:13]([CH2:12][S:6][C:4]1[N:3]=[C:2]([SH:7])[S:1][CH:5]=1)(=[NH:14])[NH2:15]

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 27769572-Chloroacetamidine monohydrochlorideHCID 47394282,4-Thiazolidinedithione

生成物 1

HCID 178479362HCID 178479362、化合物収率 19.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

In 20 ml of ethanol was suspended 1.49 g of thiazolidine -2,4-dithione, and 20 ml of 1N-sodium hydroxide solution was added under ice-cooling and stirring. To the mixture was added 1.29 g of α-chloroacetamidine hydrochloride, and the resultant was stirred at room temperature for 2.5 hours and concentrated. The precipitating crystals were collected by filtration, suspended to water, and hydrochloric acid was added to the suspension to dissolve the crystals. Thereafter this solution was subjected to a column chromatography on XAD-II (450 ml) being eluted with water. The eluate was evaporated to dryness and treated with ethanol. The resultant crystals were washed with a (1:2) mixture of ethanol and ethyl acetate to give 0.48 g of 4-amidinomethylthio-2-mercaptothiazole hydrochloride as colorless crystals. mp 178°-181° C. (decomp.)

後処理

  1. additionwas added under ice-
  2. temperaturecooling
  3. stirringthe resultant was stirred at room temperature for 2.5 hours
  4. concentrationconcentrated
  5. filtrationThe precipitating crystals were collected by filtration
  6. additionwas added to the suspension
  7. dissolutionto dissolve the crystals
  8. washbeing eluted with water
  9. customThe eluate was evaporated to dryness
  10. additiontreated with ethanol
  11. washThe resultant crystals were washed with a (1:2) mixture of ethanol and ethyl acetate

出典と根拠

ORDレコード
ord-2427e4b4d2aa4c52b5a2a490dcb1af75
出典データセット
uspto-grants-1990_11
特許番号
US04971963

反応ノート

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