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Pyridine → (4aR,7aS)-6-(5-Fluoropyrimidin-2-yl)-7a-phenyl-4,4a,5,7-tetrahydropyrrolo[3,4-d][1,3]thiazin-2-amine

HRID 470273
ノート
印刷プレビュー

反応式

HRID 470273 の反応式
N1C=CC=CC=1.[F:7][C:8]1[CH:9]=[N:10][C:11]([N:14]2[CH2:22][C@@H:21]3[C@@:16]([C:32]4[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=4)([N:17]=[C:18]([NH:23]C(=O)C4C=CC=CC=4)[S:19][CH2:20]3)[CH2:15]2)=[N:12][CH:13]=1.Cl.CON>C(O)C>[F:7][C:8]1[CH:13]=[N:12][C:11]([N:14]2[CH2:22][C@@H:21]3[C@@:16]([C:32]4[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=4)([N:17]=[C:18]([NH2:23])[S:19][CH2:20]3)[CH2:15]2)=[N:10][CH:9]=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 1049PyridineHCID 521874O-Methylhydroxylamine hydrochlorideHCID 86762233N-[(4aR,7aS)-6-(5-Fluoropyrimidin-2-yl)-7a-phenyl-4,4a,5,7-tetrahydropyrrolo[3,4-d][1,3]thiazin-2-yl]benzamide

生成物 1

HCID 78318759(4aR,7aS)-6-(5-Fluoropyrimidin-2-yl)-7a-phenyl-4,4a,5,7-tetrahydropyrrolo[3,4-d][1,3]thiazin-2-amine

試薬・触媒・溶媒 1

HCID 702Ethanol
溶媒

反応条件

温度
60 °C

実験手順

Pyridine (20 mL, 197 mmol) is added to a mixture of N-[(4aR,7aS)-6-(5-fluoropyrimidin-2-yl)-7a-phenyl-4,4a,5,7-tetrahydropyrrolo[3,4-d][1,3]thiazin-2-yl]benzamide (9.5 g, 22 mmol), O-methylhydroxylamine hydrochloride (15 g, 175 mmol) in ethanol (85 mL) and the mixture is stirred at 60° C. for 2 hours. The mixture is cooled to ambient temperature and concentrated. The mixture is diluted with water (100 mL) and ethyl acetate (100 mL) and the pH to 2 using 1 M hydrochloric acid. The aqueous layer is separated and the pH is adjusted to 10 using 2 M sodium hydroxide. The resulting aqueous solution is extracted with ethyl acetate (2×100 mL). The organic layers are combined, dried over magnesium sulfate, filtered, and concentrated. The crude product is purified over silica gel using a 5% solution of dichloromethane/2 M ammonia in methanol. Chiral Analysis of the product; column: Chiralpak AD 0.46×15 cm, 5 μm; eluent: 100% (methanol with 0.2% dimethylethylamine); flow: 0.75 ml/min at UV 254 nm; Rt=6.9 minutes. (4.6 g, 64%, >98% ee). ES/MS (m/e): 330 (M+H).

後処理

  1. temperatureThe mixture is cooled to ambient temperature
  2. concentrationconcentrated
  3. additionThe mixture is diluted with water (100 mL) and ethyl acetate (100 mL)
  4. customThe aqueous layer is separated
  5. extractionThe resulting aqueous solution is extracted with ethyl acetate (2×100 mL)
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe crude product is purified over silica gel using a 5% solution of dichloromethane/2 M ammonia in methanol

出典と根拠

ORDレコード
ord-b96efea5742744269a176c9d100652f3
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08629270B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート