Ammonia → 3-(2-Bromo-13-chloro-6-methyl-8alpha-ergolinyl)-1,1-diethylurea

HRID 35858

반응식

HRID 35858 반응식
[Br:1][C:2]1[NH:16][C:15]2[C:17]3[C:3]=1[CH2:4][C@@H:5]1[C@@H:10]([C:11]=3[CH:12]=[CH:13][CH:14]=2)[CH2:9][C@H:8]([NH:18][C:19](=[O:25])[N:20]([CH2:23][CH3:24])[CH2:21][CH3:22])[CH2:7][N:6]1[CH3:26].[Cl:27]N1C(=O)N(Cl)C(=O)N(Cl)C1=O.N.ClCCl>FC(F)(F)C(O)=O>[Br:1][C:2]1[NH:16][C:15]2[C:17]3[C:3]=1[CH2:4][C@@H:5]1[C@@H:10]([C:11]=3[CH:12]=[C:13]([Cl:27])[CH:14]=2)[CH2:9][C@H:8]([NH:18][C:19](=[O:25])[N:20]([CH2:23][CH3:24])[CH2:21][CH3:22])[CH2:7][N:6]1[CH3:26]

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 6344DichloromethaneHCID 6909Trichloroisocyanuric AcidHCID 130598603-(2-Bromo-6-methyl-8alpha-ergolinyl)-1,1-diethylurea

생성물 1

HCID 677885733-(2-Bromo-13-chloro-6-methyl-8alpha-ergolinyl)-1,1-diethylurea

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

2.1 g of 3-(2-bromo-6-methyl-8alpha-ergolinyl)-1,1-diethylurea (5 mmol) and 388 mg of trichloroisocyanuric acid (1.67 mmol) are dissolved in 100 ml of trifluoroacetic acid at room temperature. After 15 minutes, ice is added, it is made alkaline with conc. ammonia and shaken out with dichloromethane. The organic phases are dried and concentrated by evaporation, the residue is chromatographed and the product crystallizes from ethyl acetate/ether, yield 480 mg (21% of theory).

후처리

  1. additionice is added
  2. customThe organic phases are dried
  3. concentrationconcentrated by evaporation
  4. customthe residue is chromatographed
  5. customthe product crystallizes from ethyl acetate/ether, yield 480 mg (21% of theory)

출처 및 근거

ORD 기록
ord-e4f87c257b9c434bb882cda9bcf99f6e
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05411966

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