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Sodium Methoxide → N-(4-{(E)-2-[3-tert-Butyl-2-methoxy-5-(6-methoxy-2-oxo-1,2-dihydro-pyridin-3-yl)-phenyl]-vinyl}-3-methoxymethyl-phenyl)-methanesulfonamide

HRID 2390858
ノート
印刷プレビュー

反応式

HRID 2390858 の反応式
Br[CH2:2][C:3]1[CH:4]=[C:5]([NH:32][S:33]([CH3:36])(=[O:35])=[O:34])[CH:6]=[CH:7][C:8]=1/[CH:9]=[CH:10]/[C:11]1[CH:16]=[C:15]([C:17]2[C:18](=[O:25])[NH:19][C:20]([O:23][CH3:24])=[CH:21][CH:22]=2)[CH:14]=[C:13]([C:26]([CH3:29])([CH3:28])[CH3:27])[C:12]=1[O:30][CH3:31].[CH3:37][O-:38].[Na+]>CO>[C:26]([C:13]1[C:12]([O:30][CH3:31])=[C:11](/[CH:10]=[CH:9]/[C:8]2[CH:7]=[CH:6][C:5]([NH:32][S:33]([CH3:36])(=[O:34])=[O:35])=[CH:4][C:3]=2[CH2:2][O:38][CH3:37])[CH:16]=[C:15]([C:17]2[C:18](=[O:25])[NH:19][C:20]([O:23][CH3:24])=[CH:21][CH:22]=2)[CH:14]=1)([CH3:28])([CH3:29])[CH3:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 10942334Sodium MethoxideHCID 68540957N-(3-bromomethyl-4-{(E)-2-[3-tert-butyl-2-methoxy-5-(6-methoxy-2-oxo-1,2-dihydro-pyridin-3-yl)-phenyl]-vinyl}-phenyl)-methanesulfonamide

生成物 1

HCID 67070255N-(4-{(E)-2-[3-tert-Butyl-2-methoxy-5-(6-methoxy-2-oxo-1,2-dihydro-pyridin-3-yl)-phenyl]-vinyl}-3-methoxymethyl-phenyl)-methanesulfonamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

step 3—A solution of 324 (93 mg, 0.162 mmol) in MeOH (10 mL) and sodium methoxide (10 mL, 5 mmol, 0.5 M methanol solution) was stirred at RT overnight. The reaction mixture was concentrated, diluted with EtOAc and acidified with 6N HCl (1 mL). The organic extract was dried (Na2SO4), filtered and concentrated. The crude product was purified on a preparative TLC plate developed with 2:1 EtOAc/hexane to afford 26 mg (31%) of I-209 as an off-white solid.

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additiondiluted with EtOAc
  3. extractionThe organic extract
  4. dry with materialwas dried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe crude product was purified on a preparative TLC plate
  8. customto afford 26 mg (31%) of I-209 as an off-white solid

出典と根拠

ORDレコード
ord-4a339d8984fd40bdb99933a83cd87412
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08273773B2

反応ノート

読み込み中…

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