Potassium Carbonate → HCID 58277434、化合物

HRID 1949225ノート

反応式

HRID 1949225 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:8]2[C:12]([C:13]3[CH:18]=[CH:17][CH:16]=[C:15]([OH:19])[CH:14]=3)=[CH:11][C:10]([C:20]([O:22][CH2:23][CH3:24])=[O:21])=[N:9]2)[CH:5]=[CH:6][CH:7]=1.C(=O)([O-])[O-].[K+].[K+].[C:31]([O:34][CH2:35][CH2:36][CH2:37]Br)(=[O:33])[CH3:32]>CN(C=O)C>[C:31]([O:34][CH2:35][CH2:36][CH2:37][O:19][C:15]1[CH:14]=[C:13]([C:12]2[N:8]([C:4]3[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[CH:3]=3)[N:9]=[C:10]([C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH:11]=2)[CH:18]=[CH:17][CH:16]=1)(=[O:33])[CH3:32]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 122357751-Propanol, 3-bromo-, 1-acetateHCID 58277403HCID 58277403、化合物

生成物 1

HCID 58277434HCID 58277434、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

100 mg (0.292 mmol) of the compound of Example 44A are provided in 1 ml of dry DMF, 242 mg (1.75 mmol) of potassium carbonate and 158 mg (0.875 mmol) of 1-acetoxy-3-bromopropane are added, and the mixture is stirred at 90° C. for 4 h. The reaction mixture is subsequently purified by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient with the addition of 0.1% formic acid) and 109 mg (84% of theory) of the title compound are obtained.

後処理

  1. customThe reaction mixture is subsequently purified by preparative HPLC (RP18 column
  2. additionmobile phase: acetonitrile/water gradient with the addition of 0.1% formic acid) and 109 mg (84% of theory) of the title compound
  3. customare obtained

出典と根拠

ORDレコード
ord-966fe6118a2042e798728aa9a0cb331c
出典データセット
uspto-grants-2013_03
特許番号
US08399682B2

反応ノート

読み込み中…