[3-(2-Amino-3-nitro-phenylcarbamoyl)-propyl]methyl-carbamic acid tert-butyl ester → methyl-[3-(4-nitro-1H-benzoimidazol-2-yl)-propyl]-carbamic acid tert-butyl ester

HRID 220281

反応式

HRID 220281 の反応式
[C:1]([O:5][C:6](=[O:25])[N:7]([CH2:9][CH2:10][CH2:11][C:12](=O)[NH:13][C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[C:15]=1[NH2:23])[CH3:8])([CH3:4])([CH3:3])[CH3:2]>C(O)(=O)C>[C:1]([O:5][C:6](=[O:25])[N:7]([CH3:8])[CH2:9][CH2:10][CH2:11][C:12]1[NH:13][C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[C:15]=2[N:23]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

3

反応物 1

HCID 68412474[3-(2-Amino-3-nitro-phenylcarbamoyl)-propyl]methyl-carbamic acid tert-butyl ester

生成物 1

HCID 68412537methyl-[3-(4-nitro-1H-benzoimidazol-2-yl)-propyl]-carbamic acid tert-butyl ester収率 91%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 4.4 g of [3-(2-amino-3-nitro-phenylcarbamoyl)-propyl]methyl-carbamic acid tert-butyl ester in 36 mL of acetic acid was heated at 90° C. for 5 h and concentrated in vacuo. The residue was taken up in DCM, washed with sat. NaHCO3 solution, dried over anh. Na2SO4 and concentrated in vacuo to yield 3.8 g of methyl-[3-(4-nitro-1H-benzoimidazol-2-yl)-propyl]-carbamic acid tert-butyl ester as dark yellow oil.

後処理

  1. concentrationconcentrated in vacuo
  2. washwashed with sat. NaHCO3 solution
  3. dry with materialdried over anh. Na2SO4
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-4aded8f57dda4ab0a40aa39f5dd8194c
出典データセット
uspto-grants-2012_06
特許番号
US08202885B2

関連ノート

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