Water → HCID 68589889、化合物

HRID 472753ノート

反応式

HRID 472753 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 68589889HCID 68589889、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

(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.

後処理

  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)

出典と根拠

ORDレコード
ord-ff2e07721b4a48c8a7fdcf452ab50b8a
出典データセット
uspto-grants-2014_01
特許番号
US08633211B2

反応ノート

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