Carbon Tetrachloride → HCID 21848394、化合物

HRID 2082578ノート

反応式

HRID 2082578 の反応式
[CH2:1]([O:3][C:4]([CH2:6][NH:7][C:8](=[O:19])[CH2:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([CH2:17]O)=[CH:13][CH:12]=1)=[O:5])[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:40]>C(Cl)Cl>[CH2:1]([O:3][C:4]([CH2:6][NH:7][C:8](=[O:19])[CH2:9][O:10][C:11]1[CH:16]=[CH:15][C:14]([CH2:17][Cl:40])=[CH:13][CH:12]=1)=[O:5])[CH3:2]

参加物

5

反応物 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 21848389N-(ethoxycarbonylmethyl)-2-(4-hydroxymethylphenoxy)acetamide

生成物 1

HCID 21848394HCID 21848394、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of N-(ethoxycarbonylmethyl)-2-(4-hydroxymethylphenoxy)acetamide (3.96 g), triphenylphosphine (3.88 g), carbon tetrachloride (10 ml) and methylene chloride (20 ml) was heated at reflux for 1.5 hours. The reaction mixture was evaporated under reduced pressure, and ethyl acetate was added to the residue. After removal of the insolubles by filtration, the filtrate was chromatographed on silica gel column (eluent; ethyl acetate), and the desired fractions were collected and recrystallized from ethyl acetate/ether to give N-(ethoxycarbonylmethyl)-2-(4-chloromethylphenoxy)acetamide (2.8 g).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 1.5 hours
  3. customThe reaction mixture was evaporated under reduced pressure, and ethyl acetate
  4. additionwas added to the residue
  5. customAfter removal of the insolubles
  6. filtrationby filtration
  7. customthe filtrate was chromatographed on silica gel column (eluent; ethyl acetate)
  8. customthe desired fractions were collected
  9. customrecrystallized from ethyl acetate/ether

出典と根拠

ORDレコード
ord-72354a5aad0c4fdd8c688b63daf71ec5
出典データセット
uspto-grants-1993_02
特許番号
US05189211

反応ノート

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