Triethylamine → 2-Chloro-n-ethyl-n-(1-methylheptyl)-6-(trimethylsilyl)benzamide

HRID 610908

반응식

HRID 610908 반응식
C(N(CC)CC)C.[Cl:8][C:9]1[CH:17]=[CH:16][CH:15]=[C:14]([Si:18]([CH3:21])([CH3:20])[CH3:19])[C:10]=1[C:11](Cl)=[O:12].[CH2:22]([NH:24][CH:25]([CH3:32])[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])[CH3:23]>C1(C)C=CC=CC=1>[Cl:8][C:9]1[CH:17]=[CH:16][CH:15]=[C:14]([Si:18]([CH3:21])([CH3:20])[CH3:19])[C:10]=1[C:11]([N:24]([CH2:22][CH3:23])[CH:25]([CH3:32])[CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31])=[O:12]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 5250531-Heptanamine, 1-methyl, N-ethylHCID 151835572-Chloro-6-(trimethylsilyl)benzoyl chloride

생성물 1

HCID 186301442-Chloro-n-ethyl-n-(1-methylheptyl)-6-(trimethylsilyl)benzamide수율 38%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Triethylamine (2.02 g, 20 mmol) was added to a mixture of the compound of Example b (2.47 g, 10 mmol) and N-ethyl-N-(1-methylhept-1-yl)amine (3.15 g, 20 mmol) in toluene (25 mL). The reaction was stirred 2.5 h at ambient temperature, then was partitioned between ethyl acetate and dilute citric acid. The organic phase was washed twice with sat aq NaHCO3, followed with brine, then was dried (MgSO4), concentrated, and kugelrohr distilled under vacuum. The fraction which distilled at 157° C. was collected to afford 1.16 g of the title compound as an amber oil, a 38% yield.

후처리

  1. customwas partitioned between ethyl acetate and dilute citric acid
  2. washThe organic phase was washed twice with sat aq NaHCO3
  3. dry with materialwas dried (MgSO4)
  4. concentrationconcentrated
  5. distillationkugelrohr distilled under vacuum
  6. distillationThe fraction which distilled at 157° C.
  7. customwas collected

출처 및 근거

ORD 기록
ord-0c5cadf687cb49138e072c7e031be4a3
출처 데이터셋
uspto-grants-1999_12
특허 번호
US05998466

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