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

HRID 35858

反応式

HRID 35858 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-e4f87c257b9c434bb882cda9bcf99f6e
出典データセット
uspto-grants-1995_05
特許番号
US05411966

関連ノート

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