Dimethylformamide → 2-(4-Chlorophenyl)-3-methylbutanamide

HRID 894949노트

반응식

HRID 894949 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH:12]([CH3:14])[CH3:13])[C:9](O)=[O:10])=[CH:4][CH:3]=1.C(Cl)(=O)C(Cl)=O.C[N:22](C)C=O>CCOCC>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH:12]([CH3:14])[CH3:13])[C:9]([NH2:22])=[O:10])=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 16197Benzeneacetic acid, 4-chloro-alpha-(1-methylethyl)-HCID 65578Oxalyl chloride

생성물 1

HCID 128981762-(4-Chlorophenyl)-3-methylbutanamide

시약·촉매·용매 1

HCID 3283Diethyl Ether촉매

실험 절차

To a solution of 4.25 g (20 mmol) of 2-(4-chlorophenyl)-3-methylbutanoic acid in 30 ml of ether containing one drop of N,N-dimethylformamide is added dropwise 3.81 g (30 mmol) of oxalyl chloride. The solution is stirred at RT until gas evolution ceases. The solvent and excess oxalyl chloride ae removed in vacuo and the residue is taken up in 30 ml of ether. This solution is then added dropwise at 0°-5° to 4.86 g (40 mmol) of a 14% w/w aqueous solution of ammonia. After stirring the mixture for 30 minutes at 0°-5°, the aqueous layer is removed. The ethereal solution is washed with water, dried over sodium sulfate, filtered and concentrated in vacuo to obtain 2-(4-chlorophenyl)-3-methylbutyramide.

후처리

  1. customThe solvent and excess oxalyl chloride ae removed in vacuo
  2. additionThis solution is then added dropwise at 0°-5° to 4.86 g (40 mmol) of a 14% w/w aqueous solution of ammonia
  3. stirringAfter stirring the mixture for 30 minutes at 0°-5°
  4. customthe aqueous layer is removed
  5. washThe ethereal solution is washed with water
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-926e91f1e7bf4042a69051d8520fc82f
출처 데이터셋
uspto-grants-1981_08
특허 번호
US04285879

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