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Hydrochloric Acid → HCID 54761405、化合物

HRID 1746255
ノート
印刷プレビュー

反応式

HRID 1746255 の反応式
[C:1]1([C:7]2[O:11][C:10]([C:12]([F:15])([F:14])[F:13])=[C:9]([C:16](Cl)=[O:17])[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[F:19][C:20]([F:33])([F:32])[C:21]1[CH:22]=[C:23]([NH2:31])[CH:24]=[C:25]([C:27]([F:30])([F:29])[F:28])[CH:26]=1.C(N(CC)C(C)C)(C)C.Cl.C([O-])(O)=O.[Na+]>ClCCl>[F:19][C:20]([F:32])([F:33])[C:21]1[CH:22]=[C:23]([NH:31][C:16]([C:9]2[CH:8]=[C:7]([C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)[O:11][C:10]=2[C:12]([F:15])([F:14])[F:13])=[O:17])[CH:24]=[C:25]([C:27]([F:28])([F:30])[F:29])[CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 9480Benzenamine, 3,5-bis(trifluoromethyl)-HCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 534353995-Phenyl-2-(trifluoromethyl)-3-furancarbonyl chloride

生成物 1

HCID 54761405HCID 54761405、化合物収率 92.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

An excess of 5-phenyl-2-trifluoromethyl-furan-3-carbonyl chloride (1 g, 3.6 mmol) was added to a solution of 3,5-bis-trifluoromethyl-phenylamine (0.758 g, 3.3 mmol) and N,N-diisopropylethylamine (0.58 mL) in dichloromethane (50 mL). After stirring at room temperature for 1 day, the reaction underwent an aqueous acidic (dilute HCl, 2×30 mL) and basic (dilute NaHCO3, 2×30 mL) workup followed by washing with brine (saturated NaCl, 2×30 mL), drying over MgSO4, and concentration. The crude compound was purified by passing through a silica gel plug eluting with ethyl acetate/hexanes (2:1) to afford the title compound (1.42 g, 92% yield). ES-MS negative Q1 (m/z) 466.

後処理

  1. washby washing with brine (saturated NaCl, 2×30 mL)
  2. dry with materialdrying over MgSO4, and concentration
  3. customThe crude compound was purified
  4. washeluting with ethyl acetate/hexanes (2:1)

出典と根拠

ORDレコード
ord-91915a3060b64bbbbc89327831d10eb4
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09149527B2

反応ノート

読み込み中…

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