Methanol → HCID 21941479, 화합물

HRID 2216628노트

반응식

HRID 2216628 반응식
[N:1]1[N:9]2[C:4]([O:5][CH2:6][CH2:7][CH2:8]2)=[CH:3][C:2]=1[C:10]([O-])=[O:11].[BH4-].[Li+].CO>C1COCC1>[NH:1]1[N:9]2[CH:4]([O:5][CH2:6][CH:7]=[CH:8]2)[CH2:3][CH:2]1[CH2:10][OH:11]

참가 물질

5

반응물 3

HCID 887MethanolHCID 4148881Lithium borohydrideHCID 21941385HCID 21941385, 화합물

생성물 1

HCID 21941479HCID 21941479, 화합물수율 67%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To the stirred solution of 6,7-dihydro-5H-pyrazolo[5,1-b][1,3]oxazine-2-carboxylate: (4.0 g, 20 mmol) of in 100 ml of THF was added 0.71 g of lithium borohydride and 1.03 g of methanol. The solution was heated at 40 C. for 2.5 hour. The reaction was quenched by 1N HCl, and adjusted to pH 1.3 and stirred at room temperature for 1 hour. The reaction mixture was adjusted pH to 8 with k2CO3. The reaction mixture was extracted with ethyl acetate. The organic layer was dried over MgSO4, and concentrated to an oil and column chromatographyed to give 2.08 g of the desired product (67%); (M+H) 155.

후처리

  1. temperatureThe solution was heated at 40 C
  2. customThe reaction was quenched by 1N HCl
  3. extractionThe reaction mixture was extracted with ethyl acetate
  4. dry with materialThe organic layer was dried over MgSO4
  5. concentrationconcentrated to an oil and column

출처 및 근거

ORD 기록
ord-7456ec4eea5549179c7ad5465221eba7
출처 데이터셋
uspto-grants-2006_09
특허 번호
US07112582B2

반응 노트

불러오는 중…