Pyrazole → 1-(6-Methylergolin-8beta-ylmethyl)pyrazole

HRID 986526ノート

反応式

HRID 986526 の反応式
[H-].[Na+].[NH:3]1[CH:7]=[CH:6][CH:5]=[N:4]1.S(C1C=CC(C)=CC=1)(O[CH2:12][C@@H:13]1[CH2:27][C@H:26]2[C@@H:16]([CH2:17][C:18]3[C:28]4[C:21](=[CH:22][CH:23]=[CH:24][C:25]2=4)[NH:20][CH:19]=3)[N:15]([CH3:29])[CH2:14]1)(=O)=O>CN(C)C=O>[CH3:29][N:15]1[C@H:16]2[C@@H:26]([C:25]3[CH:24]=[CH:23][CH:22]=[C:21]4[C:28]=3[C:18]([CH2:17]2)=[CH:19][NH:20]4)[CH2:27][C@@H:13]([CH2:12][N:3]2[CH:7]=[CH:6][CH:5]=[N:4]2)[CH2:14]1

参加物

5

反応物 3

HCID 1048PyrazoleHCID 24758Sodium hydrideHCID 139330156-Methylergolin-8beta-ylmethyl tosylate

生成物 1

HCID 100637651-(6-Methylergolin-8beta-ylmethyl)pyrazole収率 91.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

0.7 g of 50% sodium hydride in an oil was added in small portions to a mixture of 2.5 g of pyrazole and 20 ml of dimethylformamide, and the resulting mixture was stirred for 30 minutes. 2.5 g of 6-methylergolin-8β-ylmethyl tosylate was added to the mixture which was then heated on a water bath for 1 hour. The solvent was distilled off under reduced pressure, and water was added to the residue. The precipitated crystals were separated by filtration, washed with water and recrystallized from dichloromethane-isopropyl ether to obtain 1.7 g of the titled compound as colorless flakes having a melting point of 192°-194° C.

後処理

  1. temperaturewas then heated on a water bath for 1 hour
  2. distillationThe solvent was distilled off under reduced pressure, and water
  3. additionwas added to the residue
  4. customThe precipitated crystals were separated by filtration
  5. washwashed with water
  6. customrecrystallized from dichloromethane-isopropyl ether

出典と根拠

ORDレコード
ord-67ff8f4531cc4717ad8d4e56c8a8ed56
出典データセット
uspto-grants-1987_12
特許番号
US04713457

反応ノート

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