Triethylamine → tert-butyl N-[(2-aminophenyl)methyl]carbamate

HRID 1872904

反応式

HRID 1872904 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4][NH2:5].C(N(CC)CC)C.O1CCOCC1.[C:23](=O)([O:29]C(C)(C)C)[O:24][C:25]([CH3:28])([CH3:27])[CH3:26]>O1CCOCC1.O.C(OCC)(=O)C>[C:25]([O:24][C:23]([NH:5][CH2:4][C:3]1[CH:6]=[CH:7][CH:8]=[CH:9][C:2]=1[NH2:1])=[O:29])([CH3:28])([CH3:27])[CH3:26]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 312751,4-DioxaneHCID 1780962-(Aminomethyl)anilineHCID 10219638Carbonic acid, bis(1,1-dimethylethyl) ester

生成物 1

HCID 4409487tert-butyl N-[(2-aminophenyl)methyl]carbamate

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 218864351,4-Dioxane--water (1/1)溶媒

実験手順

2-Aminobenzylamine (5.0 g, 40.9 mmol) and triethylamine (4.1 g, 40.9 mmol) were dissolved in a mixed solvent (50 ml) of dioxane-water (2:1). A dioxane solution (8.9 g/10 ml) of di-t-butyl carbonate was added dropwise to the solution under cooling with ice water. The mixture was stirred for 2 hours as it was. After the reaction mixture was diluted with ethyl acetate, an aqueous phase was removed, and an organic phase was washed 3 times with water and once with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was crystallized from diisopropyl ether-hexane to obtain 6.70 g of the title compound.

後処理

  1. customan aqueous phase was removed
  2. washan organic phase was washed 3 times with water
  3. dry with materialonce with saturated brine, and dried over anhydrous magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe residue was crystallized from diisopropyl ether-hexane

出典と根拠

ORDレコード
ord-80c123cac2ce4e6d842d744bad8d81a3
出典データセット
uspto-grants-2000_08
特許番号
US06110967

関連ノート

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