Methanol → {4H,5H,6H-pyrrolo[1,2-b]pyrazol-2-yl}methanol

HRID 2216562노트

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HRID 2216562 반응식
CO.[Li+].[BH4-].C([O:7][C:8]([C:10]1[CH:11]=[C:12]2[CH2:17][CH2:16][CH2:15][N:13]2[N:14]=1)=O)C>C1COCC1>[N:14]1[N:13]2[CH2:15][CH2:16][CH2:17][C:12]2=[CH:11][C:10]=1[CH2:8][OH:7]

참가 물질

5

반응물 3

HCID 887MethanolHCID 4148881Lithium borohydrideHCID 12841166ethyl 5,6-dihydro-4H-pyrrolo[1,2-b]pyrazole-2-carboxylate

생성물 1

HCID 21941359{4H,5H,6H-pyrrolo[1,2-b]pyrazol-2-yl}methanol수율 78.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
40 °C

실험 절차

MeOH (2.73 mL) was added to the THF (180 mL) solution of LiBH4 (1.63 g) under a nitrogen atmosphere at room temperature, and then 5,6-dihydro-4H-pyrrolo[1,2-b]pyrazole-2-carboxylic acid ethyl ester (8.11 g) was added to the suspension and stirred for 2 h at 40° C. The mixture was quenched with 1 mol/L HCl at pH 1 and stirred for 1 h at room temperature. Solid K2CO3 was added to the solution to adjust pH to 8 and the mixture was extracted with AcOEt. The organic layer was dried (MgSO4) and filtered. The filtrate was concentrated under reduced pressure to afford the title compound as brown crystals (4.87 g, 78%).

후처리

  1. customThe mixture was quenched with 1 mol/L HCl at pH 1
  2. stirringstirred for 1 h at room temperature
  3. additionSolid K2CO3 was added to the solution
  4. extractionthe mixture was extracted with AcOEt
  5. dry with materialThe organic layer was dried (MgSO4)
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e461a98178ca47eabce1802bc11fb8d3
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07112582B2

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