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

HRID 986523ノート

反応式

HRID 986523 の反応式
[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

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c12106e00eed45cba9a84785d133a144
出典データセット
uspto-grants-1987_12
特許番号
US04713457

反応ノート

読み込み中…