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

HRID 569315

반응식

HRID 569315 반응식
[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]

참가 물질

5

반응물 3

HCID 769Bicarbonate IonHCID 120273N-IodosuccinimideHCID 443951Terguride

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-020ebe24f10d4021b1ffeb30870c8fa2
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04731367

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