Triethylamine → HCID 178512424, 화합물

HRID 1073813노트

반응식

HRID 1073813 반응식
[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]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 27769572-Chloroacetamidine monohydrochlorideHCID 178418558HCID 178418558, 화합물

생성물 1

HCID 178512424HCID 178512424, 화합물수율 36.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7931e3afdf424e2a9c8b6c6f4e805a7c
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04971963

반응 노트

불러오는 중…