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Diisopropylethylamine → HCID 86646070、化合物

HRID 1800673
ノート
印刷プレビュー

反応式

HRID 1800673 の反応式
[C:1]([C:3]([C:6]1[CH:7]=[C:8]([CH:21]=[CH:22][CH:23]=1)[C:9]([NH:11][C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([NH:18][CH:19]=O)[CH:13]=1)=[O:10])([CH3:5])[CH3:4])#[N:2].C(N(C(C)C)C(C)C)C.ClC1[N:39]=[C:38]([S:40][C:41]#[N:42])[C:37]([N+:43]([O-:45])=[O:44])=[CH:36][N:35]=1.C(=O)([O-])O.[Na+]>O1CCCC1>[C:1]([C:3]([C:6]1[CH:7]=[C:8]([C:9]([NH:11][C:12]2[CH:13]=[C:14]([NH:18][C:19]3[N:39]=[C:38]([S:40][C:41]#[N:42])[C:37]([N+:43]([O-:45])=[O:44])=[CH:36][N:35]=3)[CH:15]=[CH:16][CH:17]=2)=[O:10])[CH:21]=[CH:22][CH:23]=1)([CH3:5])[CH3:4])#[N:2]
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 4

HCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 210775882-Chloro-5-nitropyrimidin-4-yl thiocyanateHCID 86646069HCID 86646069、化合物

生成物 1

HCID 86646070HCID 86646070、化合物収率 84%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

To a solution of 3-(1-cyano-1-methylethyl)-N-[3-(formylamino)phenyl]benzamide (676 mg, 2.42 mmol) in tetrahydrofuran (10 mL) were added N-ethyl-N-isopropylpropane-2-amine (643 μL, 3.63 mmol) and 2-chloro-5-nitropyrimidin-4-yl thiocyanate (576 mg, 2.66 mmol), and the mixture was stirred at room temperature for 30 min. To the reaction mixture was added saturated aqueous sodium hydrogen carbonate solution (30 mL), and the mixture was extracted with ethyl acetate (30 mL, 10 mL). The combined organic layer was washed with saturated brine (5 mL), and dried over anhydrous sodium sulfate. The insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was washed with ethyl acetate to give the title compound (933 mg, 84%) as a yellow solid.

後処理

  1. extractionthe mixture was extracted with ethyl acetate (30 mL, 10 mL)
  2. washThe combined organic layer was washed with saturated brine (5 mL)
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationThe insoluble material was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. washThe obtained residue was washed with ethyl acetate

出典と根拠

ORDレコード
ord-a171c67e1ab842728d161b438fbed340
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08344135B2

反応ノート

読み込み中…

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