Methanol → ethyl 2-((N-(butyloxycarbonyl)-N-methylsulfamoyl)amino)acetate

HRID 492014

反応式

HRID 492014 の反応式
CO.[C:3]1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH2:22]([O:26][C:27]([NH:29][S:30]([NH:33][CH2:34][C:35]([O:37][CH2:38][CH3:39])=[O:36])(=[O:32])=[O:31])=[O:28])[CH2:23][CH2:24][CH3:25].CC(OC(/N=N/C(OC(C)C)=O)=O)C>C1COCC1>[CH2:22]([O:26][C:27]([N:29]([CH3:3])[S:30]([NH:33][CH2:34][C:35]([O:37][CH2:38][CH3:39])=[O:36])(=[O:31])=[O:32])=[O:28])[CH2:23][CH2:24][CH3:25]

参加物

6

反応物 4

HCID 887MethanolHCID 11776TriphenylphosphineHCID 5363146Diisopropyl azodicarboxylateHCID 18449914ethyl 2-((N-(butyloxycarbonyl)sulfamoyl)amino)acetate

生成物 1

HCID 18449912ethyl 2-((N-(butyloxycarbonyl)-N-methylsulfamoyl)amino)acetate

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

To a solution of methanol (8.5 mmol) and triphenylphosphine (2.6 g, 8.5 mol) in dry THF is added a solution of ethyl 2-((N-(butyloxycarbonyl)sulfamoyl)amino)acetate from the previous step (2.4 g, 8.5 mol) and DIAD (2.0 g, 8.5 mmol) in dry THF dropwise at 0° C. under N2 atmosphere. The mixture is stirred at 0° C. for 2 h, warmed to RT and is stirred overnight. After the solvent is removed in vacuo, the residue is purified by column chromatography to afford ethyl 2-((N-(butyloxycarbonyl)-N-methylsulfamoyl)amino)acetate.

後処理

  1. temperaturewarmed to RT
  2. stirringis stirred overnight
  3. customAfter the solvent is removed in vacuo
  4. customthe residue is purified by column chromatography

出典と根拠

ORDレコード
ord-cb334018ecbf43fda115944cc9dfa34b
出典データセット
uspto-grants-2009_05
特許番号
US07531566B2

関連ノート

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