Water → HCID 22249795、化合物

HRID 966034ノート

反応式

HRID 966034 の反応式
[Br:1]Br.[O:3]1[C:7]([C:8]2[C:9]([CH3:26])=[N:10][N:11]3[C:16]4[N:17]([CH:20]([CH2:23][CH3:24])[CH2:21][CH3:22])[CH2:18][CH2:19][C:15]=4[C:14]([CH3:25])=[N:13][C:12]=23)=[CH:6][C:5]2[CH:27]=[CH:28][CH:29]=[CH:30][C:4]1=2.O>CN(C)C=O.C(OCC)(=O)C>[Br:1][C:6]1[C:5]2[CH:27]=[CH:28][CH:29]=[CH:30][C:4]=2[O:3][C:7]=1[C:8]1[C:9]([CH3:26])=[N:10][N:11]2[C:16]3[N:17]([CH:20]([CH2:21][CH3:22])[CH2:23][CH3:24])[CH2:18][CH2:19][C:15]=3[C:14]([CH3:25])=[N:13][C:12]=12

参加物

6

反応物 3

HCID 962WaterHCID 24408BromineHCID 22249918HCID 22249918、化合物

生成物 1

HCID 22249795HCID 22249795、化合物収率 96.7%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Bromine (1.0 M solution in carbon tetrachloride 0.3 mL, 0.30 mmol) was added to a solution of 3-benzo[b]furan-2-yl-8-(1-ethylpropyl)-2,5-dimethyl-7,8-dihydro-6H-pyrazolo[1,5-a]pyrrolo[3,2-e]pyrimidine (50 mg, 0.13 mmol) in N,N-dimethylformamide (0.3 mL) at 0° C., followed by stirring for one hour. Hypo water was added thereto, and the mixture was diluted with ethyl acetate, washed with an aqueous saturated solution of ammonium chloride and brine, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (10% ethyl acetate/hexane), to give the title compound (57 mg) as white crystals.

後処理

  1. washwashed with an aqueous saturated solution of ammonium chloride and brine
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customevaporated
  4. customThe residue was purified by silica gel column chromatography (10% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-8a19a511e5e84a68907b56a7efb24184
出典データセット
uspto-grants-2005_10
特許番号
US06951865B2

反応ノート

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