Water → HCID 22249918、化合物

HRID 966033ノート

反応式

HRID 966033 の反応式
Br[C:2]1[C:3]([CH3:20])=[N:4][N:5]2[C:10]3[N:11]([CH:14]([CH2:17][CH3:18])[CH2:15][CH3:16])[CH2:12][CH2:13][C:9]=3[C:8]([CH3:19])=[N:7][C:6]=12.[O:21]1[C:25]([Sn](CCCC)(CCCC)CCCC)=[CH:24][C:23]2[CH:39]=[CH:40][CH:41]=[CH:42][C:22]1=2.C(OCC)(=O)C.O>CN(C)C=O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[O:21]1[C:25]([C:2]2[C:3]([CH3:20])=[N:4][N:5]3[C:10]4[N:11]([CH:14]([CH2:17][CH3:18])[CH2:15][CH3:16])[CH2:12][CH2:13][C:9]=4[C:8]([CH3:19])=[N:7][C:6]=23)=[CH:24][C:23]2[CH:39]=[CH:40][CH:41]=[CH:42][C:22]1=2

参加物

7

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 38258561-benzofuran-2-yl(tributyl)stannaneHCID 22249888HCID 22249888、化合物

生成物 1

HCID 22249918HCID 22249918、化合物収率 33.3%

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒HCID 6228Dimethylformamide溶媒

実験手順

A solution of 3-bromo-8-(1-ethylpropyl)-2,5-dimethyl-7,8-dihydro-6H-pyrazolo[1,5-a]pyrrolo[3,2-e]pyrimidine (300 mg, 0.89 mmol), benzo[b]furan-2-yl(tributyl)tin (0.72 g, 1.78 mmol) and Pd(PPh3)4 (103 mg, 0.90 mmol) in N,N-dimethylformamide (15 mL) was stirred at 120° C. for one day. Ethyl acetate and water were added thereto, followed by filtering through Celite. The organic layer of the filtrate was washed with brine, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by silica gel column chromatography (0-5% ethyl acetate/hexane), to give the title compound (111 mg) as white crystals.

後処理

  1. filtrationby filtering through Celite
  2. washThe organic layer of the filtrate was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customevaporated
  5. customThe residue was purified by silica gel column chromatography (0-5% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-3b3ff42cd4eb40a1a054f9224aa78be8
出典データセット
uspto-grants-2005_10
特許番号
US06951865B2

反応ノート

読み込み中…