Methane → N-(6-methylergolin-8beta-ylmethyl)succinimide

HRID 986530ノート

反応式

HRID 986530 の反応式
[H-].[Na+].[C:3]1(=[O:9])[NH:7][C:6](=[O:8])[CH2:5][CH2:4]1.S(C1C=CC(C)=CC=1)(O[CH2:14][C@@H:15]1[CH2:29][C@H:28]2[C@@H:18]([CH2:19][C:20]3[C:30]4[C:23](=[CH:24][CH:25]=[CH:26][C:27]2=4)[NH:22][CH:21]=3)[N:17]([CH3:31])[CH2:16]1)(=O)=O.C>C(O)C.CN(C)C=O>[CH3:31][N:17]1[C@H:18]2[C@@H:28]([C:27]3[CH:26]=[CH:25][CH:24]=[C:23]4[C:30]=3[C:20]([CH2:19]2)=[CH:21][NH:22]4)[CH2:29][C@@H:15]([CH2:14][N:7]2[C:6](=[O:8])[CH2:5][CH2:4][C:3]2=[O:9])[CH2:16]1

参加物

7

反応物 4

HCID 297MethaneHCID 11439SuccinimideHCID 24758Sodium hydrideHCID 139330156-Methylergolin-8beta-ylmethyl tosylate

生成物 1

HCID 10246462N-(6-methylergolin-8beta-ylmethyl)succinimide収率 54.8%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 6228Dimethylformamide溶媒

実験手順

0.8 g of 50% sodium hydride in an oil was added in small portions to a mixture of 3.4 g of succinimide and 50 ml of dimethylformamide, and the resulting mixture was stirred for 30 minutes. 2.0 g of 6-methylergolin-8β-ylmethyl tosylate was added to the mixture which was then heated on a water bath for 30 minutes. The solvent was distilled off under reduced pressure, and water was added to the residue. The precipitated crystals were separated by filtration, and washed with water. The crystals thus obtained were treated with charcoal in ethanol and recrystallized from ethanol to obtain 0.9 g of the titled compound as colorless needles having a melting point of 233°-238° C. (with decomposition).

後処理

  1. temperaturewas then heated on a water bath for 30 minutes
  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. customThe crystals thus obtained
  7. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-ea454ccb77b3439989efa0917448d450
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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