Triethylamine → HCID 178512424、化合物

HRID 1073813ノート

反応式

HRID 1073813 の反応式
[SH:1][C:2]1[S:3][C:4]([SH:7])=[N:5][N:6]=1.C(N(CC)CC)C.Cl.Cl[CH2:17][C:18]([NH2:20])=[NH:19]>CN(C=O)C>[C:18]([CH2:17][S:1][C:2]1[S:3][C:4]([SH:7])=[N:5][N:6]=1)(=[NH:19])[NH2:20]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 27769572-Chloroacetamidine monohydrochlorideHCID 178418558HCID 178418558、化合物

生成物 1

HCID 178512424HCID 178512424、化合物収率 36.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of 1.50 g of 2,5-dimercapto-1,3,4-thiadiazole and 4.2 ml of triethylamine in 30 ml of DMF was added 1.29 g of α-chloroacetamidine hydrochloride at room temperature under stirring. Further, the mixture was stirred for 2.5 hours at room temperature and concentrated under reduced pressure. The residue was subjected to a column chromatography on silica gel (100 g), eluting with a (4:1) mixture of acetonitrile and water. The pertinent fractions were collected and concentrated under reduced pressure, and the concentrate was subjected to a column chromatography on XAD-II (450 ml) being washed with water, and eluted with 10% aqueous ethanol. After concentrating, the precipitating crystals were filtered to give 755mg of 2-amidinomethylthio-5-mercapto-1,3,4-thiadiazole as colorless crystals, mp: 184°-187° C.

後処理

  1. stirringFurther, the mixture was stirred for 2.5 hours at room temperature
  2. concentrationconcentrated under reduced pressure
  3. washeluting with a (4:1) mixture of acetonitrile and water
  4. customThe pertinent fractions were collected
  5. concentrationconcentrated under reduced pressure
  6. washbeing washed with water
  7. washeluted with 10% aqueous ethanol
  8. concentrationAfter concentrating
  9. filtrationthe precipitating crystals were filtered

出典と根拠

ORDレコード
ord-7931e3afdf424e2a9c8b6c6f4e805a7c
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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