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Hydrochloric Acid → HCID 24960268、化合物

HRID 1947001
ノート
印刷プレビュー

反応式

HRID 1947001 の反応式
Cl.O1[C:6]2([CH2:11][CH2:10][CH:9]([NH:12][C:13]3[N:18]=[C:17]([N:19]4[C:27]5[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=5)[CH:21]=[N:20]4)[CH:16]=[CH:15][N:14]=3)[CH2:8][CH2:7]2)[O:5]CC1.[OH-].[Na+]>C1COCC1>[N:19]1([C:17]2[CH:16]=[CH:15][N:14]=[C:13]([NH:12][CH:9]3[CH2:8][CH2:7][C:6](=[O:5])[CH2:11][CH2:10]3)[N:18]=2)[C:27]2[C:22](=[CH:23][CH:24]=[CH:25][CH:26]=2)[CH:21]=[N:20]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 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 24960269HCID 24960269、化合物

生成物 1

HCID 24960268HCID 24960268、化合物収率 102.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
80 °C

実験手順

Aqueous HCl (3 M, 40 mL) was added to (1,4-dioxaspiro[4.5]dec-8-yl)-(4-indazol-1-yl-pyrimidin-2-yl)-amine (1.89 g, 5 mmol) in THF (40 mL), and the resulting mixture heated to 80° C. for 1 h. The reaction mixture was cooled and poured onto a mixture of ice and aqueous NaOH (1 M, 120 mL), and the resulting suspension filtered. The collected solids were washed with water, taken up in DCM/MeOH, and a portion of the solvent evaporated under reduced pressure. The resulting suspension was filtered, the collected solids washed with hexanes, and dried under reduced pressure to give 4-(4-indazol-1-ylpyrimidin-2-ylamino)-cyclohexanone (1.57 g, 95% yield) as a white powder. MS=308 [M+H]+; MP=211.8-213.2° C.

後処理

  1. temperatureThe reaction mixture was cooled
  2. filtrationthe resulting suspension filtered
  3. washThe collected solids were washed with water
  4. customa portion of the solvent evaporated under reduced pressure
  5. filtrationThe resulting suspension was filtered
  6. washthe collected solids washed with hexanes
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-c920e918d86e4778bdf268c0f0c25940
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399462B2

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