Water → 3-Bromo-7-[(2-chloro-4-fluorophenyl)carbonyl]-2-(trifluoromethyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine

HRID 1893426ノート

反応式

HRID 1893426 の反応式
[Cl:1][C:2]1[C:7]([C:8](F)([F:10])F)=C[CH:5]=[CH:4][C:3]=1[C:12]([N:14]1[CH2:19][CH2:18][N:17]2[CH:20]=[C:21]([C:23]([F:26])([F:25])[F:24])[N:22]=[C:16]2[CH2:15]1)=O.C1C(=O)N([Br:34])C(=O)C1.[OH2:35].S([O-])([O-])=O.[Na+].[Na+]>CN(C)C=O.C(OCC)(=O)C>[Br:34][C:20]1[N:17]2[CH2:18][CH2:19][N:14]([C:12]([C:3]3[CH:4]=[CH:5][C:8]([F:10])=[CH:7][C:2]=3[Cl:1])=[O:35])[CH2:15][C:16]2=[N:22][C:21]=1[C:23]([F:25])([F:26])[F:24]

参加物

7

反応物 4

HCID 962WaterHCID 24437Sodium SulfiteHCID 67184N-bromobutanimideHCID 497850117-{[2-Chloro-3-(trifluoromethyl)phenyl]carbonyl}-2-(trifluoromethyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine

生成物 1

HCID 497853723-Bromo-7-[(2-chloro-4-fluorophenyl)carbonyl]-2-(trifluoromethyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

7-{[2-Chloro-3-(trifluoromethyl)phenyl]carbonyl}-2-(trifluoromethyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyrazine (I22) (181 mg, 0.455 mmol) was dissolved in N,N-dimethylformamide (DMF) (2 mL) and treated with NBS (97 mg, 0.546 mmol). The solution was stirred at RT for 16 h. The mixture was poured on to water (100 ml) containing 1% sodium sulfite (w/w) and extrated in to ethyl acetate (3×50 ml). Combined extracts were washed with brine (50 ml), dried over anhydrous sodium sulfate and concentrated to afford crude product. The crude product was purified by MDAP to afford desired product in 135 mg.

後処理

  1. washCombined extracts were washed with brine (50 ml)
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated
  4. customto afford crude product
  5. customThe crude product was purified by MDAP

出典と根拠

ORDレコード
ord-ea9dd6c2c7a24d3aadbdb9f88f0a3a50
出典データセット
uspto-grants-2013_08
特許番号
US08513248B2

反応ノート

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