Triethylamine → N-(2-methylcyclohexyl)-3-fluoro-4-(2-propynyloxy)benzamide

HRID 601992

반응식

HRID 601992 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][C:10]=1[O:11][CH2:12][C:13]#[CH:14])[C:5](Cl)=[O:6].[CH3:15][CH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH:17]1[NH2:22].C(N(CC)CC)C>C(OCC)(=O)C>[CH3:15][CH:16]1[CH2:21][CH2:20][CH2:19][CH2:18][CH:17]1[NH:22][C:5](=[O:6])[C:4]1[CH:8]=[CH:9][C:10]([O:11][CH2:12][C:13]#[CH:14])=[C:2]([F:1])[CH:3]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 234322-MethylcyclohexylamineHCID 574456843-Fluoro-4-(2-propynyloxy)benzoyl chloride

생성물 1

HCID 57445691N-(2-methylcyclohexyl)-3-fluoro-4-(2-propynyloxy)benzamide수율 93.1%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

To a mixture of 5 ml of ethyl acetate and 0.30 g of 3-fluoro-4-(2-propynyloxy)benzoyl chloride were added 0.19 g of 2-methylcyclohexylamine and 0.20 g of triethylamine in order at room temperature. The mixture obtained was stirred at room temperature for 1 hour. Then, ethyl acetate was added to the reaction mixture and the mixture was filtered through Celite. The filtrate was concentrated under reduced pressure. The residue was washed in order with methyl tert-butyl ether and hexane to obtain 0.38 g of N-(2-methylcyclohexyl)-3-fluoro-4-(2-propynyloxy)benzamide (hereinafter, described as the compound 34 of the present invention) represented by the formula:

후처리

  1. customThe mixture obtained
  2. filtrationthe mixture was filtered through Celite
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. washThe residue was washed in order with methyl tert-butyl ether and hexane

출처 및 근거

ORD 기록
ord-d708bf979a894f9eb57e9f66ceeec4d0
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902400B2

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