Triethylamine → HCID 178485068、化合物

HRID 1702473ノート

反応式

HRID 1702473 の反応式
[CH3:1][C:2]1[NH:6][CH:5]=[N:4][C:3]=1[CH2:7][S:8][CH2:9][CH2:10][NH2:11].C(N(CC)CC)C.[C:19]([NH:21][C:22](Cl)=[N:23][CH3:24])#[N:20]>CO>[C:19]([N:21]=[C:22]([NH:11][CH2:10][CH2:9][S:8][CH2:7][C:3]1[N:4]=[CH:5][NH:6][C:2]=1[CH3:1])[NH:23][CH3:24])#[N:20]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 6655684-(((2-Aminoethyl)thio)methyl)-5-methylimidazoleHCID 12918610N-cyano-N'-methylchloroformamidine

生成物 1

HCID 178485068HCID 178485068、化合物収率 22.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a stirred solution of 2-(5-methylimidazol-4-ylmethylthio)ethylamine (1.0 g) and triethylamine (0.71 g) in methanol (20 ml) was added N-cyano-N'-methylchloroformamidine (0.82 g) and stirred for 7.5 hrs. at 50°-55° C. After evaporation, the residue was subjected to chromatography on SiO2 [eluant: CHCl3 -MeOH (10:1)]. The resulting crude product was added to water (3 ml) and extracted repeatedly with ethyl acetate. Ethyl acetate extracts were dried over anhydrous MgSO4 and concentrated under a reduced pressure to small volume. The resulting crystals were collected by filtration and washed with ethyl acetate to give N"-cyano-N-methyl-N'-[2-(5-methylimidazol-4-ylmethylthio)ethyl]guanidine (0.33 g). Yield 22.4%, m.p. 134°-137° C.

後処理

  1. customat 50°-55° C
  2. customAfter evaporation
  3. additionThe resulting crude product was added to water (3 ml)
  4. extractionextracted repeatedly with ethyl acetate
  5. dry with materialEthyl acetate extracts were dried over anhydrous MgSO4
  6. concentrationconcentrated under a reduced pressure to small volume
  7. filtrationThe resulting crystals were collected by filtration
  8. washwashed with ethyl acetate

出典と根拠

ORDレコード
ord-ab700c3708cf4166b010fdbf2e849a44
出典データセット
uspto-grants-1983_04
特許番号
US04381395

反応ノート

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