Triethylamine → HCID 178485068, 화합물

HRID 1702473노트

반응식

HRID 1702473 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 178485068HCID 178485068, 화합물수율 22.4%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ab700c3708cf4166b010fdbf2e849a44
출처 데이터셋
uspto-grants-1983_04
특허 번호
US04381395

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