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Triethylamine → 3-chloro-N-(3-(4-(1-(2-cyano-1-cyclopropylethyl)-1H-pyrazol-4-yl)-5-methoxypyrimidin-2-ylamino)phenyl)propane-1-sulfonamide

HRID 1876902
ノート
印刷プレビュー

反応式

HRID 1876902 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([NH:8][C:9]2[N:14]=[C:13]([C:15]3[CH:16]=[N:17][N:18]([CH:20]([CH:24]4[CH2:26][CH2:25]4)[CH2:21][C:22]#[N:23])[CH:19]=3)[C:12]([O:27][CH3:28])=[CH:11][N:10]=2)[CH:5]=[CH:6][CH:7]=1.O1CCOCC1.C(N(CC)CC)C.[Cl:42][CH2:43][CH2:44][CH2:45][S:46](Cl)(=[O:48])=[O:47]>>[Cl:42][CH2:43][CH2:44][CH2:45][S:46]([NH:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([NH:8][C:9]2[N:14]=[C:13]([C:15]3[CH:16]=[N:17][N:18]([CH:20]([CH:24]4[CH2:26][CH2:25]4)[CH2:21][C:22]#[N:23])[CH:19]=3)[C:12]([O:27][CH3:28])=[CH:11][N:10]=2)[CH:3]=1)(=[O:48])=[O:47]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 8471TriethylamineHCID 154103-Chloropropanesulphonyl chlorideHCID 312751,4-DioxaneHCID 580145283-(4-{2-[(3-aminophenyl)amino]-5-methoxypyrimidin-4-yl}-1H-pyrazol-1-yl)-3-cyclopropylpropanenitrile

生成物 1

HCID 687551903-chloro-N-(3-(4-(1-(2-cyano-1-cyclopropylethyl)-1H-pyrazol-4-yl)-5-methoxypyrimidin-2-ylamino)phenyl)propane-1-sulfonamide

実験手順

To a mixture of 3-(4-{2-[(3-aminophenyl)amino]-5-methoxypyrimidin-4-yl}-1H-pyrazol-1-yl)-3-cyclopropylpropanenitrile (prepared according to Example 345, 8.0 mg, 0.000021 mol) in 1,4-dioxane (0.1 mL, 0.002 mol) was added triethylamine (0.02 mL, 0.0001 mol), followed by 3-chloropropane-1-sulfonyl chloride (0.0039 mL, 0.000032 mol). The reaction was stirred at room temperature for 1 h, quenched with 1 N HCl. The mixture was extracted with EtOAc and the organic layer was separated. The combined organic layers were washed with brine, dried over MgSO4, and evaporated to dryness to provide the desired sulfonylated intermediate.

後処理

  1. customquenched with 1 N HCl
  2. extractionThe mixture was extracted with EtOAc
  3. customthe organic layer was separated
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over MgSO4
  6. customevaporated to dryness
  7. customto provide the

出典と根拠

ORDレコード
ord-2f7f8639979f4b8cadb0f724efdb163a
出典データセット
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08309718B2

反応ノート

読み込み中…

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