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Triethylamine → N-{3-[4-(4-Acetyl-2-fluoro-phenyl)-piperazine-1-carbonyl]-4-morpholin-4-yl-phenyl}-methanesulfonamide

HRID 736188
ノート
印刷プレビュー

反応式

HRID 736188 の反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([N:26]2[CH2:31][CH2:30][O:29][CH2:28][CH2:27]2)=[C:6]([CH:25]=1)[C:7]([N:9]1[CH2:14][CH2:13][N:12]([C:15]2[CH:20]=[CH:19][C:18]([C:21](=[O:23])[CH3:22])=[CH:17][C:16]=2[F:24])[CH2:11][CH2:10]1)=[O:8].C(N(CC)CC)C.[CH3:39][S:40](Cl)(=[O:42])=[O:41]>O1CCOCC1.O>[C:21]([C:18]1[CH:19]=[CH:20][C:15]([N:12]2[CH2:11][CH2:10][N:9]([C:7]([C:6]3[CH:25]=[C:2]([NH:1][S:40]([CH3:39])(=[O:42])=[O:41])[CH:3]=[CH:4][C:5]=3[N:26]3[CH2:27][CH2:28][O:29][CH2:30][CH2:31]3)=[O:8])[CH2:14][CH2:13]2)=[C:16]([F:24])[CH:17]=1)(=[O:23])[CH3:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 44580511HCID 44580511、化合物

生成物 1

HCID 59793624N-{3-[4-(4-Acetyl-2-fluoro-phenyl)-piperazine-1-carbonyl]-4-morpholin-4-yl-phenyl}-methanesulfonamide収率 59%

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 31275
1,4-Dioxane
溶媒
2 回

実験手順

To a solution of 1-{4-[4-(5-Amino-2-morpholin-4-yl-benzoyl)-piperazin-1-yl]-3-fluoro-phenyl}-ethanone (50 mg, 0.12 mmol) and triethylamine (33 ul, 0.234 mmol) in dioxane (1.5 ml) was added a solution of methanesulfonyl chloride (15 mg, 0.13 mmol) in dioxane (0.5 ml). The mixture was stirred at room temperature for 3 hours. The reaction mixture was stirred in water. The yellow solid was filtered, washed with water and dissolved in CH2Cl2. The solution was dried over Na2SO4, filtered and the solvent was removed in vacuo. The residue was chromatographed over silica gel eluent: Heptane/ethyl acetate 0%-100% (5 minutes) to provide the title compound (35 mg, 59%) as a yellow solid MS (m/e): 505.3 (M+H, 100%)

後処理

  1. filtrationThe yellow solid was filtered
  2. washwashed with water
  3. dissolutiondissolved in CH2Cl2
  4. dry with materialThe solution was dried over Na2SO4
  5. filtrationfiltered
  6. customthe solvent was removed in vacuo
  7. customThe residue was chromatographed over silica gel eluent

出典と根拠

ORDレコード
ord-ccf0d462edc74dac8e8075eca00a9d8e
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07595314B2

反応ノート

読み込み中…

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