Acetyl chloride → 3-(1-Acetyl-6-methyl-13-nitro-8alpha-ergolinyl)-1,1-diethylurea

HRID 35219ノート

反応式

HRID 35219 の反応式
[N+:1]([C:4]1[CH:5]=[C:6]2[C:19]3[C:9]([CH2:10][C@@H:11]4[C@@H:16]([C:17]=3[CH:18]=1)[CH2:15][C@H:14]([NH:20][C:21](=[O:27])[N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[CH2:13][N:12]4[CH3:28])=[CH:8][NH:7]2)([O-:3])=[O:2].[C:29](Cl)(=[O:31])[CH3:30].[OH-].[K+]>C(Cl)Cl.S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.C(=O)(O)[O-].[Na+]>[C:29]([N:7]1[C:6]2[C:19]3[C:9]([CH2:10][C@@H:11]4[C@@H:16]([C:17]=3[CH:18]=[C:4]([N+:1]([O-:3])=[O:2])[CH:5]=2)[CH2:15][C@H:14]([NH:20][C:21](=[O:27])[N:22]([CH2:25][CH3:26])[CH2:23][CH3:24])[CH2:13][N:12]4[CH3:28])=[CH:8]1)(=[O:31])[CH3:30]

参加物

7

反応物 3

HCID 6367Acetyl chlorideHCID 14797Potassium HydroxideHCID 133749573-(13-Nitro-6-methyl-8alpha-ergolinyl)-1,1-diethylurea

生成物 1

HCID 867423593-(1-Acetyl-6-methyl-13-nitro-8alpha-ergolinyl)-1,1-diethylurea

試薬・触媒・溶媒 3

HCID 94433Tetrabutylammonium hydrogen sulfate触媒HCID 6344Dichloromethane溶媒HCID 516892Sodium Bicarbonate溶媒

実験手順

A solution is prepared from 410 mg of 3-(13-nitro-6-methyl-8α-ergolinyl)-1,1-diethylurea in 10 ml of methylene chloride, 40 mg of tetrabutylammonium hydrogen sulfate and 0.8 ml of acetyl chloride are added, and this mixture is poured on 1 g of pulverized potassium hydroxide. After 1.5 hours of agitation at room temperature, the mixture is diluted with sodium bicarbonate solution, the organic phase is separated and dried with sodium sulfate. After evaporation and chromatography as indicated in Example 9, 375 mg of 3-(1-acetyl-6-methyl-13-nitro-8α-ergolinyl)-1,1-diethylurea is obtained.

後処理

  1. additionare added
  2. customthe organic phase is separated
  3. dry with materialdried with sodium sulfate
  4. customAfter evaporation and chromatography

出典と根拠

ORDレコード
ord-8a99252617924af7b5e6e37583a9b8a9
出典データセット
uspto-grants-1988_08
特許番号
US04766128

反応ノート

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