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1,2-Dichloroethane → N-(4-tert-Butyl-benzyl)-2-(3,4-diamino-phenyl)-propionamide

HRID 1626864
ノート
印刷プレビュー

反応式

HRID 1626864 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([CH:9]([CH3:13])[C:10]([OH:12])=O)[CH:5]=[CH:6][C:7]=1[NH2:8].[C:14]([C:18]1[CH:25]=[CH:24][C:21]([CH2:22][NH2:23])=[CH:20][CH:19]=1)([CH3:17])([CH3:16])[CH3:15].C(Cl)CCl.C1C=CC2N(O)N=NC=2C=1.C(N(CC)CC)C>CN(C=O)C.O>[C:14]([C:18]1[CH:19]=[CH:20][C:21]([CH2:22][NH:23][C:10](=[O:12])[CH:9]([C:4]2[CH:5]=[CH:6][C:7]([NH2:8])=[C:2]([NH2:1])[CH:3]=2)[CH3:13])=[CH:24][CH:25]=1)([CH3:17])([CH3:15])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 757711-HydroxybenzotriazoleHCID 27356554-tert-ButylbenzylamineHCID 122268182-(3,4-Diaminophenyl)propanoic acid

生成物 1

HCID 57742164N-(4-tert-Butyl-benzyl)-2-(3,4-diamino-phenyl)-propionamide

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒

実験手順

2-(3,4-Diaminophenyl)propanoic acid (436 mg, 2.42 mmol) in DMF (5 mL) was added 4-t-butylbenzylamine (399 mg, 2.44 mmol), EDC (702 mg, 3.66 mmol), HOBt (496 mg, 3.67 mmol), triethylamine (617 mg, 6.10 mmol) at 0° C. The reaction mixture was stirred for 16 hours at room temperature, and then the mixture was added water (50 mL) and extracted with methylene chloride. The organic layer was dried with MgSO4 and filtered. Methylene chloride was removed by evaporation. The residue was purified by column chromatography eluting with CH2Cl2/MeOH=20/1.

後処理

  1. extractionextracted with methylene chloride
  2. dry with materialThe organic layer was dried with MgSO4
  3. filtrationfiltered
  4. customMethylene chloride was removed by evaporation
  5. customThe residue was purified by column chromatography
  6. washeluting with CH2Cl2/MeOH=20/1

出典と根拠

ORDレコード
ord-ca90899431d94a6e844499897156b422
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08785474B2

反応ノート

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