Bicarbonate Ion → 1,1-Diethyl-3-(2-iodo-6-methyl-8alpha-ergolinyl)urea

HRID 569315ノート

反応式

HRID 569315 の反応式
[CH3:1][CH2:2][N:3]([C:6]([NH:8][C@@H:9]1[CH2:24][N:23]([CH3:25])[C@H:22]2[C@@H:11]([C:12]3[C:17]4[C:18]([CH2:21]2)=[CH:19][NH:20][C:16]=4[CH:15]=[CH:14][CH:13]=3)[CH2:10]1)=[O:7])[CH2:4][CH3:5].[I:26]N1C(=O)CCC1=O.C(=O)(O)[O-]>O1CCOCC1>[CH2:4]([N:3]([CH2:2][CH3:1])[C:6]([NH:8][C@H:9]1[CH2:10][C@H:11]2[C@@H:22]([CH2:21][C:18]3[C:17]4[C:16](=[CH:15][CH:14]=[CH:13][C:12]2=4)[NH:20][C:19]=3[I:26])[N:23]([CH3:25])[CH2:24]1)=[O:7])[CH3:5]

参加物

5

反応物 3

HCID 769Bicarbonate IonHCID 120273N-IodosuccinimideHCID 443951Terguride

生成物 1

HCID 135590301,1-Diethyl-3-(2-iodo-6-methyl-8alpha-ergolinyl)urea収率 76%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A solution is prepared from 1 mmol of terguride in 20 ml of anhydrous dioxane, combined with about 1.5 ml of N-iodosuccinimide at room temperature and stirred for 30 minutes. The reaction mixture is then poured into a saturated bicarbonate solution, extracted with methylene chloride and the organic phase is dried with magnesium sulfate. After evaporation of the solvent, the residue is chromatographed on silica gel, thus obtaining in a 76% yield 1,1-diethyl-3-(2-iodo-6-methyl-8α-ergolinyl)urea.

後処理

  1. extractionextracted with methylene chloride
  2. dry with materialthe organic phase is dried with magnesium sulfate
  3. customAfter evaporation of the solvent
  4. customthe residue is chromatographed on silica gel

出典と根拠

ORDレコード
ord-020ebe24f10d4021b1ffeb30870c8fa2
出典データセット
uspto-grants-1988_03
特許番号
US04731367

反応ノート

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