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Potassium Hydroxide → (-)-7-{[5-(1-Cyclopropyl-2,2,2-trifluoro-1-hydroxyethyl)-1,3-thiazol-2-yl]thio}-4-pyridin-3-yl-2H-chromen-2-one

HRID 2116652
ノート
印刷プレビュー

反応式

HRID 2116652 の反応式
[OH-].[K+].[CH:3]1([C:6]([C:12]2[S:16][C:15]([SH:17])=[N:14][CH:13]=2)([OH:11])[C:7]([F:10])([F:9])[F:8])[CH2:5][CH2:4]1.Br[C:19]1[CH:28]=[C:27]2[C:22]([C:23]([C:30]3[CH:31]=[N:32][CH:33]=[CH:34][CH:35]=3)=[CH:24][C:25](=[O:29])[O:26]2)=[CH:21][CH:20]=1>CO>[CH:3]1([C:6]([C:12]2[S:16][C:15]([S:17][C:19]3[CH:28]=[C:27]4[C:22]([C:23]([C:30]5[CH:31]=[N:32][CH:33]=[CH:34][CH:35]=5)=[CH:24][C:25](=[O:29])[O:26]4)=[CH:21][CH:20]=3)=[N:14][CH:13]=2)([OH:11])[C:7]([F:8])([F:10])[F:9])[CH2:5][CH2:4]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 233702367-Bromo-4-(pyridin-3-yl)-2H-1-benzopyran-2-oneHCID 178519846HCID 178519846、化合物

生成物 1

HCID 11352007(-)-7-{[5-(1-Cyclopropyl-2,2,2-trifluoro-1-hydroxyethyl)-1,3-thiazol-2-yl]thio}-4-pyridin-3-yl-2H-chromen-2-one

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
120 °C

実験手順

Powdered KOH (0.111 g, 1.98 mmol) was added to a solution of (−)-1-cyclopropyl-2,2,2-trifluoro-1-(2-mercapto-1,3-thiazol-5-yl)ethanol (0.507 g, 1.98 mmol) in dry MeOH (2 mL). When a solution was obtained, the reaction mixture was concentrated to dryness. Dry toluene was then added and the mixture was concentrated to dryness again. The residue was dissolved in NMP (2 mL) and 7-bromo-4-pyridin-3-yl-2H-chromen-2-one (0.500 g, 1.65 mmol) was added and the resulting mixture was stirred at 120° C. for 16 h. Once cooled, the mixture was directly applied onto a column of silica gel and chromatographed (acetone/toluene 5:95 to 20:80), affording the title compound. 1H NMR (500 MHz, CDCl3): δ 8.76 (brd, 1H), 8.68 (d, 1H), 7.85 (s, 1H), 7.79 (brd, 1H), 7.50 (m, 2H), 7.31-7.36 (m, 2H), 6.39 (s, 1H), 3.05 (br s, 1H), 1.48 (m, 1H), 0.71 (m, 2H), 0.62 (m, 1H), 0.56 (m, 1H); [α]D=−31.1° (c=1.05, EtOH).

後処理

  1. customWhen a solution was obtained
  2. concentrationthe reaction mixture was concentrated to dryness
  3. additionDry toluene was then added
  4. concentrationthe mixture was concentrated to dryness again
  5. dissolutionThe residue was dissolved in NMP (2 mL)
  6. temperatureOnce cooled
  7. customchromatographed (acetone/toluene 5:95 to 20:80)

出典と根拠

ORDレコード
ord-97014e6d1ab648928219696b0a34db2f
出典データセット
uspto-grants-2008_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07439260B2

反応ノート

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