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Phenyl chloroformate → HCID 59379904、化合物

HRID 2353740
ノート
印刷プレビュー

反応式

HRID 2353740 の反応式
Cl[C:2]([O:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:3].[CH3:11][C@H:12]1[CH2:17][O:16][CH2:15][CH2:14][N:13]1[C:18]1[CH:23]=[C:22]([CH2:24][S:25]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=2[C:34]([F:37])([F:36])[F:35])(=[O:27])=[O:26])[N:21]=[C:20]([C:38]2[CH:44]=[CH:43][C:41]([NH2:42])=[CH:40][CH:39]=2)[N:19]=1.C(=O)([O-])O.[Na+]>O1CCOCC1.C(OCC)(=O)C>[CH3:11][C@H:12]1[CH2:17][O:16][CH2:15][CH2:14][N:13]1[C:18]1[CH:23]=[C:22]([CH2:24][S:25]([C:28]2[CH:33]=[CH:32][CH:31]=[CH:30][C:29]=2[C:34]([F:35])([F:36])[F:37])(=[O:27])=[O:26])[N:21]=[C:20]([C:38]2[CH:39]=[CH:40][C:41]([NH:42][C:2](=[O:3])[O:4][C:5]3[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=3)=[CH:43][CH:44]=2)[N:19]=1
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 15891Phenyl chloroformateHCID 516892Sodium BicarbonateHCID 593799934-[4-[(3S)-3-methylmorpholin-4-yl]-6-[[2-(trifluoromethyl)phenyl]sulfonylmethyl]pyrimidin-2-yl]aniline

生成物 1

HCID 59379904HCID 59379904、化合物収率 97.7%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒
HCID 31275
1,4-Dioxane
溶媒

実験手順

Phenyl chloroformate (0.535 mL, 4.26 mmol) was added to 4-[4-[(3S)-3-methylmorpholin-4-yl]-6-[[2-(trifluoromethyl)phenyl]sulfonylmethyl]pyrimidin-2-yl]aniline (1.4 g, 2.84 mmol) and sodium hydrogen carbonate (0.358 g, 4.26 mmol) in dioxane (20 mL) at 5° C. under nitrogen. The resulting mixture was stirred at RT for 2 hours then the reaction mixture diluted with ethyl acetate (200 mL), and washed with water (125 mL). The organic layer was dried (MgSO4), filtered and evaporated to afford crude product which was triturated with a mixture of diethyl ether and isohexane to give the desired material as a white solid (1.70 g).

後処理

  1. washwashed with water (125 mL)
  2. dry with materialThe organic layer was dried (MgSO4)
  3. filtrationfiltered
  4. customevaporated
  5. customto afford crude product which
  6. customwas triturated with a mixture of diethyl ether and isohexane

出典と根拠

ORDレコード
ord-17a5f732e241454d84e5a0cf092f8463
出典データセット
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07750003B2

反応ノート

読み込み中…

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