Potassium Carbonate → HCID 18320759、化合物

HRID 1699529

反応式

HRID 1699529 の反応式
[C:1]([C:3]1[N:4]([CH2:28][C:29]2[CH:34]=[CH:33][C:32]([O:35][CH3:36])=[CH:31][C:30]=2[O:37][CH3:38])[C:5](=[O:27])[N:6]([C:17]2[C:25]3[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=3)[N:19](C)[CH:18]=2)[C:7]=1[C:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[NH:10][CH:9]=1)#[N:2].[CH3:39][S:40]([O:43][CH2:44][CH2:45][CH2:46]OS(C)(=O)=O)(=[O:42])=[O:41].C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[CH3:39][S:40]([O:43][CH2:44][CH2:45][CH2:46][N:10]1[C:11]2[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:8]([C:7]2[N:6]([C:17]3[C:25]4[C:20](=[CH:21][CH:22]=[CH:23][CH:24]=4)[NH:19][CH:18]=3)[C:5](=[O:27])[N:4]([CH2:28][C:29]3[CH:34]=[CH:33][C:32]([O:35][CH3:36])=[CH:31][C:30]=3[O:37][CH3:38])[C:3]=2[C:1]#[N:2])=[CH:9]1)(=[O:42])=[O:41]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 275321,3-Propanediol, 1,3-dimethanesulfonateHCID 18320729HCID 18320729、化合物

生成物 1

HCID 18320759HCID 18320759、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

To a solution 0.15 g (0.298 mmol) of the product from step b) in 2 ml of DMF was 0.40 g (1.72 mmol) of 1,3-propandiol bismethansulfonate and 0.50 g (3.62 mmol) of K2CO3. The mixture was stirred at 70° C. overnight and partitioned between EtOAc and water. The organic phase was washed with water and brine and finally evaporated. The residue was purified by chromatography on silica furnishing 0.11 g (59%) of the sub-title compound.

後処理

  1. custompartitioned between EtOAc and water
  2. washThe organic phase was washed with water and brine
  3. customfinally evaporated
  4. customThe residue was purified by chromatography on silica furnishing 0.11 g (59%) of the sub-title compound

出典と根拠

ORDレコード
ord-8490e5a0de73423d845d5d859fab2c15
出典データセット
uspto-grants-2002_02
特許番号
US06346625B1

関連ノート

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