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Hydrochloric Acid → HCID 22445845, 화합물

HRID 2375350
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HRID 2375350 반응식
[C:1]1([CH2:7][CH2:8][NH:9][C:10](=[O:12])[CH3:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:13](Cl)(=[O:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.[Cl-].[Cl-].[Cl-].[Al+3].Cl>[N+](C1C=CC=CC=1)([O-])=O>[C:13]([C:4]1[CH:5]=[CH:6][C:1]([CH2:7][CH2:8][NH:9][C:10](=[O:12])[CH3:11])=[CH:2][CH:3]=1)(=[O:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 7412Benzoyl chlorideHCID 70143N-(2-phenylethyl)acetamideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 22445845HCID 22445845, 화합물수율 34.3%

시약·촉매·용매 1

HCID 7416Nitrobenzene용매2회

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온도
50 °C

실험 절차

N-(2-Phenylethyl)acetamide (49.01 mmol, 8.00 g) was introduced into nitrobenzene (40 ml). Benzoyl chloride (54.07 mmol, 7.60 g) was added thereto and then, at room temperature, aluminum tri-chloride (73.52 mmol, 9.80 g) was introduced in portions. The mixture was then heated at 50° C. for 8 h. The reaction mixture was poured into a mixture of ice and concentrated hydrochloric acid, and nitrobenzene was removed by steam distillation. The aqueous residue was extracted with ethyl acetate. The residue after concentration of the organic phase was chromatographed on silica gel (mobile phase dichloromethane/methanol (3% by volume)), resulting in 4.5 g of the title compound as orange oil.

후처리

  1. customwas removed by steam distillation
  2. extractionThe aqueous residue was extracted with ethyl acetate
  3. customThe residue after concentration of the organic phase was chromatographed on silica gel (mobile phase dichloromethane/methanol (3% by volume))

출처 및 근거

ORD 기록
ord-cbb5fc12478c4562bac866e9c577c191
출처 데이터셋
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07465744B2

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