Imidazole → 1-(6-Methylergolin-8beta-ylmethyl)imidazole

HRID 986523노트

반응식

HRID 986523 반응식
[H-].[Na+].[NH:3]1[CH:7]=[CH:6][N:5]=[CH:4]1.CN(C)C=O.S(C1C=CC(C)=CC=1)(O[CH2:17][C@@H:18]1[CH2:32][C@H:31]2[C@@H:21]([CH2:22][C:23]3[C:33]4[C:26](=[CH:27][CH:28]=[CH:29][C:30]2=4)[NH:25][CH:24]=3)[N:20]([CH3:34])[CH2:19]1)(=O)=O>C(O)C>[CH3:34][N:20]1[C@H:21]2[C@@H:31]([C:30]3[CH:29]=[CH:28][CH:27]=[C:26]4[C:33]=3[C:23]([CH2:22]2)=[CH:24][NH:25]4)[CH2:32][C@@H:18]([CH2:17][N:3]2[CH:7]=[CH:6][N:5]=[CH:4]2)[CH2:19]1

참가 물질

6

반응물 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 139330156-Methylergolin-8beta-ylmethyl tosylate

생성물 1

HCID 100637641-(6-Methylergolin-8beta-ylmethyl)imidazole수율 58.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1.0 g of 50% sodium hydride in an oil was added in small portions to a mixture of 2.0 g of imidazole and 20 ml of dimethylformamide, and the resulting mixture was stirred for 30 minutes. 3.0 g of 6-methylergolin-8β-ylmethyl tosylate was added to the mixture which was then heated on a water bath for 3 hours. After allowing the mixture to cool, ice-water was added to the reaction mixture, and the precipitated crystals were filtered and washed with water. The crystals thus obtained were dissolved in ethanol, and the solution was concentrated to a volume of about 1/3, followed by allowing to cool to obtain 1.3 g of the titled compound as colorless prisms having a melting point of higher than 260° C. (with decomposition).

후처리

  1. temperaturewas then heated on a water bath for 3 hours
  2. temperatureto cool
  3. filtrationthe precipitated crystals were filtered
  4. washwashed with water
  5. customThe crystals thus obtained
  6. concentrationthe solution was concentrated to a volume of about 1/3
  7. temperatureto cool

출처 및 근거

ORD 기록
ord-c12106e00eed45cba9a84785d133a144
출처 데이터셋
uspto-grants-1987_12
특허 번호
US04713457

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