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Water → HCID 71765537, 화합물

HRID 2272964
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HRID 2272964 반응식
Cl[CH2:2][C:3]1[CH:23]=[C:6]2[C:7](=[O:22])[NH:8][C:9]([C:11]3[CH:16]=[CH:15][C:14]([O:17][C:18]([F:21])([F:20])[F:19])=[CH:13][CH:12]=3)=[CH:10][N:5]2[N:4]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>C1COCC1>[CH3:2][C:3]1[CH:23]=[C:6]2[C:7](=[O:22])[NH:8][C:9]([C:11]3[CH:12]=[CH:13][C:14]([O:17][C:18]([F:21])([F:20])[F:19])=[CH:15][CH:16]=3)=[CH:10][N:5]2[N:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 71765536HCID 71765536, 화합물

생성물 1

HCID 71765537HCID 71765537, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 18.9 mg (0.055 mmol) 2-chloromethyl-6-(4-trifluoromethoxy-phenyl)-5H-pyrazolo[1,5-a]pyrazin-4-one in 0.5 ml THF is flushed with nitrogen. 3.5 mg (0.092 mmol) Lithiumaluminiumhydride is added and the reaction mixture is stirred for 5 hours at room temperature. Then 1 ml THF, 3.5 μl water, 3.5 μl 15% aqueous NaOH solution and 10.5 μl water are added successively. The resulting suspension is stirred for 30 minutes at room temperature. The precipitate is filtered off and washed with THF and ethanol. The filtrate is evaporated and purified by preparative HPLC to give 2-methyl-6-(4-trifluoromethoxy-phenyl)-5H-pyrazolo[1,5-a]pyrazin-4-one as colourless crystals; HPLC/MS 2.53 min (B), [M+H] 310;

후처리

  1. stirringThe resulting suspension is stirred for 30 minutes at room temperature
  2. filtrationThe precipitate is filtered off
  3. washwashed with THF and ethanol
  4. customThe filtrate is evaporated
  5. custompurified by preparative HPLC

출처 및 근거

ORD 기록
ord-2056aa1e3a7d4d1781ee29e2e9405795
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09120805B2

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