HCID 71000688、化合物 → HCID 69081573、化合物

HRID 1023455ノート

反応式

HRID 1023455 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]#[C:9][C:10]2[CH:15]=[CH:14][N:13]=[C:12]([NH:16][C:17]([NH2:19])=[O:18])[CH:11]=2)=[C:4]([CH3:20])[CH:3]=1.[H][H]>CO.C(Cl)Cl.[Pd]>[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][CH2:9][C:10]2[CH:15]=[CH:14][N:13]=[C:12]([NH:16][C:17]([NH2:19])=[O:18])[CH:11]=2)=[C:4]([CH3:20])[CH:3]=1

参加物

6

反応物 2

HCID 71000688HCID 71000688、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 69081573HCID 69081573、化合物収率 70.8%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 887Methanol溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

[4-(4-Fluoro-2-methyl-phenylethynyl)-pyridin-2-yl]-urea (25 mg, 0.093 mmol) is dissolved in methanol (1.0 mL) and DCM (1.0 mL). Then 5% palladium on carbon (20 mg, 0.0090 mmol) is added. The reaction is stirred for 16 hrs under the hydrogen atmosphere. The palladium on carbon is filtered and the filtrate is concentrated to give the crude product. Methanol (1 mL) is added into the crude and a white solid is formed. The solid is filtered, rinsed with more methanol and dried to give 18 mg of the titled product.

後処理

  1. filtrationThe palladium on carbon is filtered
  2. concentrationthe filtrate is concentrated
  3. customto give the crude product
  4. customa white solid is formed
  5. filtrationThe solid is filtered
  6. washrinsed with more methanol
  7. customdried

出典と根拠

ORDレコード
ord-487953f7d2e64fafac075067ece294c6
出典データセット
uspto-grants-2014_05
特許番号
US08722709B2

反応ノート

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