N-bromobutanimide → HCID 86653752、化合物

HRID 2189040ノート

反応式

HRID 2189040 の反応式
[C:1]([O:5][C:6](=[O:31])[CH2:7][O:8][C@H:9]1[CH2:14][CH2:13][CH2:12][C@@H:11]([O:15][C:16]2[C:17]3[C:24]([C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)=[CH:23][O:22][C:18]=3[N:19]=[CH:20][N:21]=2)[CH2:10]1)([CH3:4])([CH3:3])[CH3:2].C1C(=O)N([Br:39])C(=O)C1>ClC(Cl)(Cl)Cl>[C:1]([O:5][C:6](=[O:31])[CH2:7][O:8][C@H:9]1[CH2:14][CH2:13][CH2:12][C@@H:11]([O:15][C:16]2[C:17]3[C:24]([C:25]4[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=4)=[C:23]([Br:39])[O:22][C:18]=3[N:19]=[CH:20][N:21]=2)[CH2:10]1)([CH3:4])([CH3:2])[CH3:3]

参加物

4

反応物 2

HCID 67184N-bromobutanimide2 回HCID 86653751HCID 86653751、化合物

生成物 1

HCID 86653752HCID 86653752、化合物

試薬・触媒・溶媒 1

HCID 5943Carbon Tetrachloride溶媒

反応条件

温度
60 °C

実験手順

Suspend 100 mg (0.236 mmol) of (+/−)-cis-({3-[(5-phenylfuro[2,3-d]pyrimidin-4-yl)oxy]cyclohexyl}oxy)acetic acid tert-butyl ester in 0.2 ml of tetrachloromethane and add 46.1 mg (0.259 mmol) of NBS. Stir the reaction mixture at 60° C. for a total of 2 h, and add a further 23 mg of NBS after 1 h. After cooling, remove the tetrachloromethane under reduced pressure and purify the residue by preparative RP-HPLC (eluent: acetonitrile/water). 43.6 mg (36.8% of theory) of the target product are obtained.

後処理

  1. temperatureAfter cooling
  2. customremove the tetrachloromethane under reduced pressure
  3. custompurify the residue by preparative RP-HPLC (eluent: acetonitrile/water)
  4. custom43.6 mg (36.8% of theory) of the target product are obtained

出典と根拠

ORDレコード
ord-356d5950a43c4e6ea14fa789c2f1c291
出典データセット
uspto-grants-2012_12
特許番号
US08324222B2

反応ノート

読み込み中…