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Formaldehyde → 5-isopropyl-N-[6-(4-phenoxy-but-2-ynyloxy)-5-(2-methoxy-phenoxy)-2-pyrid in-4-yl-pyrimidin-4-yl]-2-pyridine sulfonamide

HRID 2085104
ノート
印刷プレビュー

反応式

HRID 2085104 の反応式
[CH:1]([C:4]1[CH:5]=[CH:6][C:7]([S:10]([NH:13][C:14]2[C:19]([O:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[O:27][CH3:28])=[C:18](Cl)[N:17]=[C:16]([C:30]3[CH:35]=[CH:34][N:33]=[CH:32][CH:31]=3)[N:15]=2)(=[O:12])=[O:11])=[N:8][CH:9]=1)([CH3:3])[CH3:2].[O:36]([CH2:43][C:44]#[C:45][CH2:46][OH:47])[C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1.C1(OCC#C)C=CC=CC=1.C=O.[H-].[Na+]>C1COCC1.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>[NH3:8].[CH:1]([C:4]1[CH:5]=[CH:6][C:7]([S:10]([NH:13][C:14]2[C:19]([O:20][C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=3[O:27][CH3:28])=[C:18]([O:47][CH2:46][C:45]#[C:44][CH2:43][O:36][C:37]3[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=3)[N:17]=[C:16]([C:30]3[CH:35]=[CH:34][N:33]=[CH:32][CH:31]=3)[N:15]=2)(=[O:12])=[O:11])=[N:8][CH:9]=1)([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 712FormaldehydeHCID 24758Sodium hydrideHCID 83613(Prop-2-ynyloxy)benzeneHCID 160466794-Phenoxybut-2-yn-1-olHCID 227294115-isopropyl-N-[6-chloro-5-(o-methoxyphenoxy)-2-(4-pyridyl)-4-pyrimidinyl]-2-pyridine sulfonamide

生成物 2

HCID 222Ammonia
HCID 10211514
5-isopropyl-N-[6-(4-phenoxy-but-2-ynyloxy)-5-(2-methoxy-phenoxy)-2-pyrid in-4-yl-pyrimidin-4-yl]-2-pyridine sulfonamide
収率 129%

試薬・触媒・溶媒 2

HCID 311Citric Acid溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 300 mg of 5-isopropyl-N-[6-chloro-5-(o-methoxyphenoxy)-2-(4-pyridyl)-4-pyrimidinyl]-2-pyridine sulfonamide (Example 1f) and 502 mg of 4-phenoxy-2-butyn-1-ol (prepared starting from phenyl-propargylether and para-formaldehyde following the procedure given in J. Chem. Soc. Perkin Trans. 1, 1991, 1721-1727) in 15 ml of THF was added 228 mg of 55% NaH in mineral oil. The orange suspension was stirred at room temperature for 1 h before it was diluted with 100 ml of 10% aqueous citric acid. The mixture was extracted three times with 50 ml of ethyl acetate. The combined organic phases were washed with 50 ml of water, dried over MgSO4 and evaporated. The crude product was purified by chromatography on prep. tlc-plates with ethyl acetate:methanol:sat. aqueous ammonia 8:2:1 to give 241 mg of 5-isopropyl-N-[6-(4-phenoxy-but-2-ynyloxy)-5-(2-methoxy-phenoxy)-2-pyrid in-4-yl-pyrimidin-4-yl]-2-pyridine sulfonamide as a slightly yellow foam. LC-MS: tR=5.95 min, [M+1]+=666.58, [M−1]−=664.62

後処理

  1. extractionThe mixture was extracted three times with 50 ml of ethyl acetate
  2. washThe combined organic phases were washed with 50 ml of water
  3. dry with materialdried over MgSO4
  4. customevaporated
  5. customThe crude product was purified by chromatography on prep

出典と根拠

ORDレコード
ord-6ec2f64db1c444419b3d32176712f9c1
出典データセット
uspto-grants-2004_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06720322B2

反応ノート

読み込み中…

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