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

HRID 35219노트

반응식

HRID 35219 반응식
[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]

참가 물질

7

반응물 3

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

생성물 1

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

시약·촉매·용매 3

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 6344Dichloromethane용매HCID 516892Sodium Bicarbonate용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-8a99252617924af7b5e6e37583a9b8a9
출처 데이터셋
uspto-grants-1988_08
특허 번호
US04766128

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