Potassium Carbonate → HCID 22708435、化合物

HRID 353303

反応式

HRID 353303 の反応式
[C:1]([O:5][C:6]([NH:8][C:9]1[CH:10]=[C:11]([CH2:16][CH:17]([O:23][CH2:24][CH3:25])[C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH:12]=[CH:13][C:14]=1[OH:15])=[O:7])([CH3:4])([CH3:3])[CH3:2].[CH3:26][S:27]([O:30][C:31]1[CH:36]=[CH:35][C:34]([CH2:37][CH2:38]OS(C)(=O)=O)=[CH:33][CH:32]=1)(=[O:29])=[O:28].C(=O)([O-])[O-].[K+].[K+]>CC(=O)CC>[C:1]([O:5][C:6]([NH:8][C:9]1[CH:10]=[C:11]([CH2:16][CH:17]([O:23][CH2:24][CH3:25])[C:18]([O:20][CH2:21][CH3:22])=[O:19])[CH:12]=[CH:13][C:14]=1[O:15][CH2:38][CH2:37][C:34]1[CH:33]=[CH:32][C:31]([O:30][S:27]([CH3:26])(=[O:28])=[O:29])=[CH:36][CH:35]=1)=[O:7])([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 112201221-(Methylsulfonyloxy)-2-[4-(methylsulfonyloxy)phenyl]ethaneHCID 22708408HCID 22708408、化合物

生成物 1

HCID 22708435HCID 22708435、化合物収率 21.4%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

Ethyl 3-{3-[(tert-butoxycarbonyl)amino]-4-hydroxyphenyl}-2-ethoxypropanoate (0.16 g, 0.44 mmole) and 4-{2-[(methylsulfonyl)oxy]ethyl}phenyl methanesulfonate (0.26 g, 0.88 mmole) were dissolved in 2-butanone (10 ml). Polyethyleneglycol 400 (0.05 g) and anhydrous potassium carbonate (0.092 g, 0.66 mmole) were added the mixture. After stirring at reflux for 16 hours it was checked with using HPLC whether all the starting material was consumed. The mixture was washed with water dried with magnesium sulfate and evaporated. Purification of the crude product with preparative HPLC (Kromasil C8, 7 μm, 50×250 mm) using actonitrile(60-80%) in ammonium acetate buffer (pH 7) as mobile phase gave 0.052 g (21% yield) of the desired product

後処理

  1. temperatureat reflux for 16 hours it
  2. customwas consumed
  3. washThe mixture was washed with water
  4. dry with materialdried with magnesium sulfate
  5. customevaporated
  6. customPurification of the crude product with preparative HPLC (Kromasil C8, 7 μm, 50×250 mm)

出典と根拠

ORDレコード
ord-b30695ede53f4abbae1e28d66ba39090
出典データセット
uspto-grants-2004_06
特許番号
US06750252B2

関連ノート

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