Water → 5-(3-methanesulfonylamino-phenyl)-2-methyl-thiazole-4-carboxylic Acid Methyl Ester

HRID 560259ノート

反応式

HRID 560259 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].CN1CCOCC1.[CH3:13][O:14][C:15]([C:17]1[N:18]=[C:19]([CH3:29])[S:20][C:21]=1[C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([NH2:28])[CH:23]=1)=[O:16].O>C(Cl)Cl>[CH3:13][O:14][C:15]([C:17]1[N:18]=[C:19]([CH3:29])[S:20][C:21]=1[C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([NH:28][S:2]([CH3:1])(=[O:4])=[O:3])[CH:23]=1)=[O:16]

参加物

6

反応物 4

HCID 962WaterHCID 79724-MethylmorpholineHCID 31297Methanesulfonyl chlorideHCID 66844939HCID 66844939、化合物

生成物 1

HCID 669985805-(3-methanesulfonylamino-phenyl)-2-methyl-thiazole-4-carboxylic Acid Methyl Ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Methanesulfonyl chloride (5.27 mmol) and 4-methylmorpholine (4.86 mmol) are added successively to a solution of 5-(3-amino-phenyl)-2-methyl-thiazole-4-carboxylic acid methyl ester (4.05 mmol) in DCM (50 mL). After stirring for 2 h water is added, the layers are separated and the aq. layer is extracted once with DCM. The combined organic layers are washed with citric acid (10% solution in water), dried over MgSO4 and concentrated in vacuo to give a crude product which is used without further purification. LC-MS: tR=0.84 min; [M+H]+=327.2.

後処理

  1. additionis added
  2. customthe layers are separated
  3. extractionthe aq. layer is extracted once with DCM
  4. washThe combined organic layers are washed with citric acid (10% solution in water)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e7af5bda8d874ecd8a27ad12d8806dd4
出典データセット
uspto-grants-2011_11
特許番号
US08063099B2

反応ノート

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