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

HRID 16975

반응식

HRID 16975 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
0 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-59cb70e321af4807b0cad051bb2f1012
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737283B2

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