Methanol → methyl N-(2-methyl-3-phenylbenzyl)carbamate

HRID 1168032ノート

反応式

HRID 1168032 の反応式
[CH3:1][C:2]1[C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4]Br.[O-:16][C:17]#N.[K+].CO.O.C[N:24](C)[CH:25]=[O:26]>>[CH3:1][C:2]1[C:9]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[CH:8][CH:7]=[CH:6][C:3]=1[CH2:4][NH:24][C:25](=[O:26])[O:16][CH3:17]

参加物

6

反応物 5

HCID 887MethanolHCID 962WaterHCID 6228DimethylformamideHCID 11378442Potassium cyanateHCID 147188083-(Bromomethyl)-2-methyl-1,1'-biphenyl

生成物 1

HCID 12090307methyl N-(2-methyl-3-phenylbenzyl)carbamate

実験手順

3.57 g of 2-methyl-3-phenylbenzyl bromide, 1.66 g of potassium cyanate and 7.00 g of methanol in N,N-dimethylformamide (30 ml) were stirred at 80° C. for 5 hours. After the reaction, the reaction solution was poured into water and extracted with ethyl acetate, and the organic layer was separated, dried over anhydrous magnesium sulfate and evaporated under reduced pressure for removal of the solvent. The residue was purified by silica gel column chromatography to give 2.01 g of methyl N-(2-methyl-3-phenylbenzyl)carbamate as colorless crystals. m.p. 91-94° C.

後処理

  1. customAfter the reaction
  2. extractionextracted with ethyl acetate
  3. customthe organic layer was separated
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customevaporated under reduced pressure for removal of the solvent
  6. customThe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-2fd240bb909244358f0e14dc9e319237
出典データセット
uspto-grants-2003_09
特許番号
US06620961B1

反応ノート

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