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

HRID 601992ノート

反応式

HRID 601992 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-d708bf979a894f9eb57e9f66ceeec4d0
出典データセット
uspto-grants-2011_03
特許番号
US07902400B2

反応ノート

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