Water → HCID 53981173、化合物

HRID 357087

反応式

HRID 357087 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.[N:16]1([CH:22]=[C:23]2[S:27][C:26](=[O:28])[NH:25][C:24]2=[O:29])[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1.C1CCN2C(=NCCC2)CC1.O>CN(C)C=O>[N:16]1([CH:22]=[C:23]2[S:27][C:26](=[O:28])[N:25]([CH2:2][CH2:3][CH2:4][CH2:5][S:6][C:7]3[N:12]4[CH:13]=[CH:14][N:15]=[C:11]4[CH:10]=[CH:9][CH:8]=3)[C:24]2=[O:29])[CH2:21][CH2:20][CH2:19][CH2:18][CH2:17]1

参加物

6

反応物 4

HCID 962WaterHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 18936641Imidazo[1,2-a]pyridine,5-[(4-chlorobutyl)thio]-HCID 54129473HCID 54129473、化合物

生成物 1

HCID 53981173HCID 53981173、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 241 mg (1.0 mmol) of 5-(4-chlorobutylthio)imidazo[1,2-a]pyridine and 212 mg (1.0 mmol) of 5-(piperidin-1-yl)methylene-thiazolidine-2,4-dione in 10 ml of N,N-dimethylformamide, 0.15 ml (1.0 mmol) of 1,8-diazabicyclo[5.4.0]-7-undecene was added, followed by stirring at 80° C. for 3 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, n-hexane/ethyl acetate=1/4→ethyl acetate) to yield 330 mg (79.2%, white powder) 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, n-hexane/ethyl acetate=1/4→ethyl acetate)

出典と根拠

ORDレコード
ord-dea347ba088f44a88a985b5b6558366b
出典データセット
uspto-grants-1998_11
特許番号
US05840732

関連ノート

読み込み中…