Water → HCID 18936665、化合物

HRID 357062

反応式

HRID 357062 の反応式
Cl[CH2:2][CH2:3][CH2:4][CH2:5][S:6][C:7]1[N:12]2[CH:13]=[CH:14][N:15]=[C:11]2[CH:10]=[CH:9][CH:8]=1.[NH:16]1[CH2:22][C:20](=[O:21])[NH:19][C:17]1=[O:18].C1CCN2C(=NCCC2)CC1.O>CN(C)C=O>[N:15]1[CH:14]=[CH:13][N:12]2[C:7]([S:6][CH2:5][CH2:4][CH2:3][CH2:2][N:19]3[C:20](=[O:21])[CH2:22][NH:16][C:17]3=[O:18])=[CH:8][CH:9]=[CH:10][C:11]=12

参加物

6

反応物 4

HCID 962WaterHCID 10006HydantoinHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 18936641Imidazo[1,2-a]pyridine,5-[(4-chlorobutyl)thio]-

生成物 1

HCID 18936665HCID 18936665、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

To a solution of 2.41 g (10.0 mmol) of 5-(4-chlorobutylthio)imidazo[1,2-a]pyridine and 1.00 g (10.0 mmol) of hydantoin in 30 ml of N,N-dimethylformamide, 1.50 ml (10.0 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene was added, followed by stirring at 80° C. for 16 hours. After the reaction mixture was cooled, water was added; the mixture was extracted with ethyl acetate and dried, after which the solvent was distilled off. The residue was purified by column chromatography (eluent, chloroform/methanol=20/1→10/1) to yield 1.27 g (41.7%, yellow solid) of the desired product.

後処理

  1. temperatureAfter the reaction mixture was cooled
  2. extractionthe mixture was extracted with ethyl acetate
  3. customdried
  4. distillationafter which the solvent was distilled off
  5. customThe residue was purified by column chromatography (eluent, chloroform/methanol=20/1→10/1)

出典と根拠

ORDレコード
ord-356bb265275d412ca0d7a303c808ed76
出典データセット
uspto-grants-1998_11
特許番号
US05840732

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