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Hydrochloric Acid → 2-[4-(1-aminocyclobutyl)phenyl]-N-cyclopropyl-9-fluoro-3-phenylpyrimido[1,2-b]indazol-4-amine

HRID 877055
ノート
印刷プレビュー

反応式

HRID 877055 の反応式
C(OC(=O)[NH:7][C:8]1([C:12]2[CH:17]=[CH:16][C:15]([C:18]3[C:31]([C:32]4[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=4)=[C:30]([NH:38][CH:39]4[CH2:41][CH2:40]4)[N:21]4[N:22]=[C:23]5[C:28]([CH:27]=[C:26]([F:29])[CH:25]=[CH:24]5)=[C:20]4[N:19]=3)=[CH:14][CH:13]=2)[CH2:11][CH2:10][CH2:9]1)(C)(C)C.Cl>O1CCOCC1>[NH2:7][C:8]1([C:12]2[CH:13]=[CH:14][C:15]([C:18]3[C:31]([C:32]4[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=4)=[C:30]([NH:38][CH:39]4[CH2:40][CH2:41]4)[N:21]4[N:22]=[C:23]5[C:28]([CH:27]=[C:26]([F:29])[CH:25]=[CH:24]5)=[C:20]4[N:19]=3)=[CH:16][CH:17]=2)[CH2:9][CH2:10][CH2:11]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 86702531{1-[4-(9-Fluoro-4-cyclopropylamino-3-phenyl-pyrimido[1,2-b]indazol-2-yl)phenyl]cyclobutyl}carbamic acid tert-butyl ester

生成物 1

HCID 573777662-[4-(1-aminocyclobutyl)phenyl]-N-cyclopropyl-9-fluoro-3-phenylpyrimido[1,2-b]indazol-4-amine収率 7.4%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

720 mg (1.3 mmol) Crude {1-[4-(9-fluoro-4-cyclopropylamino-3-phenyl-pyrimido[1,2-b]indazol-2-yl)phenyl]cyclobutyl}carbamic acid tert-butyl ester, described in step 2, were dissolved in 36 mL dioxane. After dropwise addition of 36 mL of a 4 M hydrogen chloride in dioxane the reaction mixture was stirred for five hours at room temperature. The reaction mixture was evaporated to dryness. Saturated aqueous sodium bicarbonate solution was added and the reaction mixture was extracted three times with ethyl acetate. The combined organic extracts were washed with brine and dried. After evaporation of the solvent the residue was purified by HPLC to yield 44.3 mg of the desired compound which was 90% pure.

後処理

  1. customThe reaction mixture was evaporated to dryness
  2. additionSaturated aqueous sodium bicarbonate solution was added
  3. extractionthe reaction mixture was extracted three times with ethyl acetate
  4. washThe combined organic extracts were washed with brine
  5. customdried
  6. customAfter evaporation of the solvent the residue
  7. customwas purified by HPLC

出典と根拠

ORDレコード
ord-6733fedc89584a859c69a313dc506941
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08987286B2

反応ノート

読み込み中…

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