Water → HCID 68589889, 화합물

HRID 472753노트

반응식

HRID 472753 반응식
[CH3:1][O:2][C:3](=[O:14])[CH2:4][NH:5][CH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[NH2:13].Cl[C:16]([O:19]C(=O)OC(Cl)(Cl)Cl)(Cl)Cl.O>O1CCOCC1>[CH3:1][O:2][C:3](=[O:14])[CH2:4][N:5]1[CH2:6][C:7]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[NH:13][C:16]1=[O:19]

참가 물질

5

반응물 3

HCID 962WaterHCID 94429TriphosgeneHCID 65440269(2-Amino-benzylamino)-acetic acid methyl ester

생성물 1

HCID 68589889HCID 68589889, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

(2-Amino-benzylamino)-acetic acid methyl ester (0.50 g, 2 mmol) and bis(trichloromethyl)carbonate (0.54 g, 2 mmol) are dissolved in dioxane (5 ml) and stirred at RT for 24 hours. The reaction mixture is treated with water and extracted with EtOAc, the organic phase is dried over MgSO4, filtered and is concentrated in vacuo. Purification by flash column chromatography on silica, eluting with DCM:MeOH (10:1) affords the title compound. [M+H]+ 221.

후처리

  1. extractionextracted with EtOAc
  2. dry with materialthe organic phase is dried over MgSO4
  3. filtrationfiltered
  4. concentrationis concentrated in vacuo
  5. customPurification by flash column chromatography on silica
  6. washeluting with DCM:MeOH (10:1)

출처 및 근거

ORD 기록
ord-ff2e07721b4a48c8a7fdcf452ab50b8a
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08633211B2

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