Diisopropylethylamine → HCID 59626733、化合物

HRID 2400375ノート

反応式

HRID 2400375 の反応式
[CH3:1]S(O)(=O)=O.[NH2:6][CH:7]1[C:21](=[O:22])[NH:20][CH2:19][C:10]2[C:11]3[CH:12]=[N:13][NH:14][C:15]=3[C:16]([Cl:18])=[CH:17][C:9]=2[CH2:8]1.C(N([CH:29]([CH3:31])[CH3:30])CC)(C)C.[C:32](=[O:35])(O)[O-:33].[Na+]>C1COCC1.O>[Cl:18][C:16]1[C:15]2[NH:14][N:13]=[CH:12][C:11]=2[C:10]2[CH2:19][NH:20][C:21](=[O:22])[CH:7]([NH:6][C:32](=[O:35])[O:33][C:29]([CH3:31])([CH3:1])[CH3:30])[CH2:8][C:9]=2[CH:17]=1

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 86649246HCID 86649246、化合物

生成物 1

HCID 59626733HCID 59626733、化合物

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒

実験手順

To a solution of 7-amino-4-chloro-6,7,9,10-tetrahydroazepino[3,4-e]indazol-8(3H)-one methanesulfonate from Step C in 1:1 THF/water (100 mL) was added diisopropyl ethylamine (1.1 g, 1.58 mL, 8.65 mmol) and Boc-anhydride (1.88 g, 8.65 mmol) and the reaction allowed to stir at room temperature for 30 minutes. The reaction was poured into a solution of saturated aqueous sodium bicarbonate and the mixture was extracted with ethyl acetate (3×100 mL). The combined organic extracts were washed once with brine (100 mL), dried over anhydrous magnesium sulfate, filtered and concentrated at reduced pressure to give 900 mg of the title compound. MS: m/z=351 (M+1).

後処理

  1. extractionthe mixture was extracted with ethyl acetate (3×100 mL)
  2. washThe combined organic extracts were washed once with brine (100 mL)
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated at reduced pressure

出典と根拠

ORDレコード
ord-d8fbffcc70fd4e8ea2be1f8ccccbd378
出典データセット
uspto-grants-2014_08
特許番号
US08796260B2

反応ノート

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