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Lithium Hydroxide → HCID 67168497, 화합물

HRID 872674
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HRID 872674 반응식
[CH3:1][S:2]([N:5]1[CH2:10][CH2:9][CH:8]([C:11]2[O:12][CH:13]=[C:14]([C:16]([O:18]CC)=[O:17])[N:15]=2)[CH2:7][CH2:6]1)(=[O:4])=[O:3].[OH-].[Li+]>C1COCC1.CO.O>[CH3:1][S:2]([N:5]1[CH2:6][CH2:7][CH:8]([C:11]2[O:12][CH:13]=[C:14]([C:16]([OH:18])=[O:17])[N:15]=2)[CH2:9][CH2:10]1)(=[O:3])=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 67169151HCID 67169151, 화합물

생성물 1

HCID 67168497HCID 67168497, 화합물수율 74.7%

시약·촉매·용매 2

HCID 962Water용매HCID 21899815MeOH tetrahydrofuran용매

실험 절차

Ethyl 2-(1-(methylsulfonyl)piperidin-4-yl)oxazole-4-carboxylate (590 mg, 1.951 mmol) was dissolved in THF/methanol mixture (9:1) and 1M lithium hydroxide (3.90 ml, 3.90 mmol) was added slowly. The reaction mixture was stirred at RT for 1 h, diluted with water and pH was adjusted to 1.5. The mixture was extracted three times with ethyl acetate. Ethyl acetate phases were combined and evaporated to yield the title compound (74.7%). 1H-NMR (400 MHz; DMSO): δ 1.68-1.81 (m, 2H), 2.06-2.15 (m, 2H), 2.85-2.96 (m, 5H), 2.99-3.10 (m, 1H), 3.51-3.59 (m, 2H), 8.67 (s, 1H), 13.02 (bs, 1H).

후처리

  1. extractionThe mixture was extracted three times with ethyl acetate
  2. customevaporated

출처 및 근거

ORD 기록
ord-013e061500ce40a6aadddfec868725af
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08975254B2

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