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Hydrochloric Acid → HCID 24960268, 화합물

HRID 1947001
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HRID 1947001 반응식
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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 24960269HCID 24960269, 화합물

생성물 1

HCID 24960268HCID 24960268, 화합물수율 102.2%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c920e918d86e4778bdf268c0f0c25940
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08399462B2

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