N-(6-(3-tert-butyl-5-(2,4-di-tert-butoxypyrimidin-5-yl)-2-vinyl phenyl)naphthalen-2-yl)methanesulfonamide → N-(6-(3-tert-butyl-5-(2,4-di-tert-butoxypyrimidin-5-yl)-2-ethyl phenyl)naphthalen-2-yl)methanesulfonamide

HRID 403686ノート

反応式

HRID 403686 の反応式
[C:1]([C:5]1[C:6]([CH:42]=[CH2:43])=[C:7]([C:27]2[CH:28]=[C:29]3[C:34](=[CH:35][CH:36]=2)[CH:33]=[C:32]([NH:37][S:38]([CH3:41])(=[O:40])=[O:39])[CH:31]=[CH:30]3)[CH:8]=[C:9]([C:11]2[C:12]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[N:13][C:14]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[N:15][CH:16]=2)[CH:10]=1)([CH3:4])([CH3:3])[CH3:2]>[Pd].CO>[C:1]([C:5]1[C:6]([CH2:42][CH3:43])=[C:7]([C:27]2[CH:28]=[C:29]3[C:34](=[CH:35][CH:36]=2)[CH:33]=[C:32]([NH:37][S:38]([CH3:41])(=[O:40])=[O:39])[CH:31]=[CH:30]3)[CH:8]=[C:9]([C:11]2[C:12]([O:22][C:23]([CH3:26])([CH3:25])[CH3:24])=[N:13][C:14]([O:17][C:18]([CH3:19])([CH3:20])[CH3:21])=[N:15][CH:16]=2)[CH:10]=1)([CH3:2])([CH3:3])[CH3:4]

参加物

4

反応物 1

HCID 66834092N-(6-(3-tert-butyl-5-(2,4-di-tert-butoxypyrimidin-5-yl)-2-vinyl phenyl)naphthalen-2-yl)methanesulfonamide

生成物 1

HCID 66833855N-(6-(3-tert-butyl-5-(2,4-di-tert-butoxypyrimidin-5-yl)-2-ethyl phenyl)naphthalen-2-yl)methanesulfonamide

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

To a 100 mL round-bottomed flask was added the product from Example 35 Part A (132 mg, 0.219 mmol), 10% palladium on carbon (20 mg, 0.019 mmol) and methanol (10 mL). The mixture was hydrogenated for 24 hours, filtered and concentrated in vacuo to give crude product which was purified by silica gel flash chromatography eluting with ethyl acetate/hexane (10% to 20%) to give the title compound.

後処理

  1. filtrationfiltered
  2. concentrationconcentrated in vacuo
  3. customto give crude product which
  4. customwas purified by silica gel flash chromatography
  5. washeluting with ethyl acetate/hexane (10% to 20%)

出典と根拠

ORDレコード
ord-eb740ff4af4843e79bfc8e76b8e59c7c
出典データセット
uspto-grants-2014_06
特許番号
US08748443B2

反応ノート

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