Lithium hydroxide, monohydrate → HCID 178503561, 화합물

HRID 1487359노트

반응식

HRID 1487359 반응식
O.[OH-].[Li+].[C:4]([C:6]1[C:7]([S:18][CH3:19])=[N:8][C:9]([OH:17])=[C:10]([CH:16]=1)[C:11]([O:13]CC)=[O:12])#[N:5]>C(O)C.O>[C:4]([C:6]1[C:7]([S:18][CH3:19])=[N:8][C:9]([OH:17])=[C:10]([CH:16]=1)[C:11]([OH:13])=[O:12])#[N:5]

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 178469059HCID 178469059, 화합물

생성물 1

HCID 178503561HCID 178503561, 화합물수율 95.1%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

4.16 g (2 eq) of lithium hydroxide monohydrate is added at room temperature to a solution of 11.8 g (49.5 mmol) of ethyl 5-cyano-2-hydroxy-6-(methylthio)nicotinate in 100 ml of ethanol and 100 ml of water. The reaction mixture is stirred at 60° C. for 2 hours. The ethanol is evaporated and 1 N aqueous soda is added. The aqueous phase is washed with ethyl acetate and then re-acidified by adding 1 N aqueous hydrogen chloride (pH=1). The precipitate formed is filtered, rinsed with water and with diethyl ether and then dried under vacuum to yield 9.9 g (95%) of 5-cyano-2-hydroxy-6-(methylthio)nicotinic acid in the form of a brown powder.

후처리

  1. customThe ethanol is evaporated
  2. addition1 N aqueous soda is added
  3. washThe aqueous phase is washed with ethyl acetate
  4. additionre-acidified by adding 1 N aqueous hydrogen chloride (pH=1)
  5. customThe precipitate formed
  6. filtrationis filtered
  7. washrinsed with water and with diethyl ether
  8. customdried under vacuum

출처 및 근거

ORD 기록
ord-af13ad3d2a1f4f4688f8bc7f48d06893
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09428510B2

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