2-[4-(4-Bromophenoxymethyl)-2,5-dioxo-imidazolidin-1-yl]-3-methyl-butyric acid methyl ester → HCID 66660886、化合物

HRID 2197271ノート

反応式

HRID 2197271 の反応式
C[O:2][C:3](=[O:29])[CH:4]([NH:8][C:9](=[O:28])[CH:10]([NH:20][C:21](OC(C)(C)C)=[O:22])[CH2:11][O:12][C:13]1[CH:18]=[CH:17][C:16]([Br:19])=[CH:15][CH:14]=1)[CH:5]([CH3:7])[CH3:6].COC(=O)C(N1C(=O)C(COC2C=CC(Br)=CC=2)NC1=O)C(C)C>Cl>[Br:19][C:16]1[CH:17]=[CH:18][C:13]([O:12][CH2:11][CH:10]2[C:9](=[O:28])[N:8]([CH:4]([CH:5]([CH3:7])[CH3:6])[C:3]([OH:2])=[O:29])[C:21](=[O:22])[NH:20]2)=[CH:14][CH:15]=1

参加物

4

反応物 2

HCID 666606712-[4-(4-Bromophenoxymethyl)-2,5-dioxo-imidazolidin-1-yl]-3-methyl-butyric acid methyl esterHCID 666609032-[3-(4-Bromophenoxy)-2-tert-butoxycarbonylamino-propionylamino]-3-methyl-butyric acid methyl ester

生成物 1

HCID 66660886HCID 66660886、化合物収率 41%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
80 °C

実験手順

A mixture of the compound obtained in step g above (22g) (759 mg, 1.907 mmol) and 3 N HCl (20 mL) was stirred at 80° C. for 2 h. The reaction mixture was cooled down and then extracted with EtOAc. The combined organic layers were dried and concentrated; the crude product was purified by silica gel column chromatography which gave the title compound as colorless oil (300 mg, 41%).

後処理

  1. temperatureThe reaction mixture was cooled down
  2. extractionextracted with EtOAc
  3. customThe combined organic layers were dried
  4. concentrationconcentrated
  5. customthe crude product was purified by silica gel column chromatography which

出典と根拠

ORDレコード
ord-98db85b568764f85b90ed13c5b86b72e
出典データセット
uspto-grants-2012_12
特許番号
US08338471B2

反応ノート

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