Triethylamine → N-(2-methylcyclopentyl)-3-fluoro-5-methoxy-4-(2-propynyloxy)benzamide

HRID 602002

反応式

HRID 602002 の反応式
Cl.[CH3:2][CH:3]1[CH2:7][CH2:6][CH2:5][CH:4]1[NH2:8].C(N(CC)CC)C.[F:16][C:17]1[CH:18]=[C:19]([CH:23]=[C:24]([O:30][CH3:31])[C:25]=1[O:26][CH2:27][C:28]#[CH:29])[C:20](Cl)=[O:21]>C(OCC)(=O)C>[CH3:2][CH:3]1[CH2:7][CH2:6][CH2:5][CH:4]1[NH:8][C:20](=[O:21])[C:19]1[CH:23]=[C:24]([O:30][CH3:31])[C:25]([O:26][CH2:27][C:28]#[CH:29])=[C:17]([F:16])[CH:18]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 191014392-Methylcyclopentan-1-amine hydrochlorideHCID 574456983-Fluoro-5-methoxy-4-(2-propynyloxy)benzoyl chloride

生成物 1

HCID 57701166N-(2-methylcyclopentyl)-3-fluoro-5-methoxy-4-(2-propynyloxy)benzamide収率 69.5%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒2 回

実験手順

To a mixture of 1 ml of ethyl acetate and 0.2 g of 2-methylcyclopentylamine hydrochloride was added 0.48 ml of triethylamine and then, a mixture of 0.24 g of 3-fluoro-5-methoxy-4-(2-propynyloxy)benzoyl chloride and 1 ml of ethyl acetate was added dropwise thereto under ice cooling. The mixture obtained was stirred at room temperature for 12 hours. Then, the reaction mixture was concentrated under reduced pressure. The residue obtained was subjected to silica gel column chromatography to obtain 0.21 g of N-(2-methylcyclopentyl)-3-fluoro-5-methoxy-4-(2-propynyloxy)benzamide (hereinafter, described as the compound 70 of the present invention) represented by the formula:

後処理

  1. additionwas added dropwise
  2. customThe mixture obtained
  3. concentrationThen, the reaction mixture was concentrated under reduced pressure
  4. customThe residue obtained

出典と根拠

ORDレコード
ord-af8ac2f70c564e48a2e22ca7b8e5209f
出典データセット
uspto-grants-2011_03
特許番号
US07902400B2

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