Dimethylformamide → 2-(2,4-Di-t-butyl phenoxy)propionyl chloride

HRID 1488906ノート

反応式

HRID 1488906 の反応式
[C:1]([C:5]1[CH:16]=[C:15]([C:17]([CH3:20])([CH3:19])[CH3:18])[CH:14]=[CH:13][C:6]=1[O:7][CH:8]([CH3:12])[C:9](O)=[O:10])([CH3:4])([CH3:3])[CH3:2].CN(C=O)C.C(Cl)(=O)C([Cl:29])=O>C(Cl)Cl>[C:1]([C:5]1[CH:16]=[C:15]([C:17]([CH3:20])([CH3:19])[CH3:18])[CH:14]=[CH:13][C:6]=1[O:7][CH:8]([CH3:12])[C:9]([Cl:29])=[O:10])([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 167740552-(2,4-Di-t-butyl phenoxy) propionic acid

生成物 1

HCID 136513232-(2,4-Di-t-butyl phenoxy)propionyl chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a stirred slurry of 2-(2,4-di-t-butyl phenoxy) propionic acid (27.8 g, 0.100 mol) in CH2Cl2 (280 mL) with 2 mL of DMF, oxalyl chloride (17.0 g, 0.134 mol) was added dropwise. The solution resulted after several minutes was stirred for 2 hr. TLC indicates no starting material. The solution was filtered through a glass wool plug to remove some debris and the filtrate was concentrated in vacuo, residue was washed with CH2Cl2 (50 mL) and was concentrated once more to give a gelatinous mixture, which was used without further purification.

後処理

  1. customThe solution resulted after several minutes
  2. filtrationThe solution was filtered through a glass wool plug
  3. customto remove some debris
  4. concentrationthe filtrate was concentrated in vacuo, residue
  5. washwas washed with CH2Cl2 (50 mL)
  6. concentrationwas concentrated once more
  7. customto give a gelatinous mixture, which
  8. customwas used without further purification

出典と根拠

ORDレコード
ord-a5cc76837bdc4e1ba6d08b6165e5aa40
出典データセット
uspto-grants-1997_10
特許番号
US05677118

反応ノート

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