Methanol → HCID 11845249, 화합물

HRID 1158870노트

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HRID 1158870 반응식
[Li+].[BH4-].CO.C([O:7][C:8]([C:10]1[CH:18]=[C:13]2[CH2:14][S:15][CH2:16][CH2:17][N:12]2[N:11]=1)=O)C>C1COCC1>[N:11]1[N:12]2[C:13]([CH2:14][S:15][CH2:16][CH2:17]2)=[CH:18][C:10]=1[CH2:8][OH:7]

참가 물질

5

반응물 3

HCID 887MethanolHCID 4148881Lithium borohydrideHCID 11845093Ethyl 6,7-dihydro-4H-pyrazolo[5,1-c][1,4]thiazine-2-carboxylate

생성물 1

HCID 11845249HCID 11845249, 화합물수율 100%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
40 °C

실험 절차

LiBH4 (cont. 90%) (536 mg) and MeOH (0.9 mL) was added to the THF (59 mL) solution of 6,7-dihydro-4H-pyrazolo[5,1-c][1,4]thiazine-2-carboxylic acid ethyl ester (3.13 g) under a nitrogen atmosphere at room temperature and stirred for 3 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 (K2CO3) and filtered. The filtrate was concentrated under reduced pressure to afford titled compound as pale yellow oil (2.51 g, quant.).

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 (K2CO3)
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-af701bb449314341948a2a84fe2046a5
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07812014B2

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