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

HRID 1488906노트

반응식

HRID 1488906 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a5cc76837bdc4e1ba6d08b6165e5aa40
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05677118

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