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Lithium hydroxide, monohydrate → HCID 178451168, 화합물

HRID 1035718
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HRID 1035718 반응식
[C:1]([O:5][C:6]([C@@H:8]1[CH2:13][CH2:12][C@H:11]([O:14][C:15]2[CH:25]=[CH:24][C:18]([C:19]([O:21]CC)=[O:20])=[CH:17][N:16]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].O.[OH-].[Li+]>C1COCC1.CO>[C:1]([O:5][C:6]([C@@H:8]1[CH2:13][CH2:12][C@H:11]([O:14][C:15]2[CH:25]=[CH:24][C:18]([C:19]([OH:21])=[O:20])=[CH:17][N:16]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:2])[CH3:3]
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참가 물질

4

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 178469088HCID 178469088, 화합물

생성물 1

HCID 178451168HCID 178451168, 화합물수율 98%

시약·촉매·용매 1

HCID 21899815MeOH tetrahydrofuran용매

실험 절차

1.33 g of ethyl cis-6-(4-tert-butoxycarbonylcyclohexyloxy)nicotinate (3.97 mmol, 1 eq.) are dissolved in 60 mL of a 1/1 mixture of THF/methanol. At 0° C., 0.333 g of lithium hydroxide monohydrate (7.93 mmol; 2 eq.) is added with stirring. After stirring for 16 hours at room temperature, the reaction medium is evaporated and aqueous 6% sulfur dioxide solution is added. The precipitate formed is filtered off and washed with water to give 1.25 g of cis-6-(4-tert-butoxycarbonylcyclohexyloxy)nicotinic acid.

후처리

  1. stirringAfter stirring for 16 hours at room temperature
  2. customthe reaction medium is evaporated
  3. additionaqueous 6% sulfur dioxide solution is added
  4. customThe precipitate formed
  5. filtrationis filtered off
  6. washwashed with water

출처 및 근거

ORD 기록
ord-898c26d57a6743d7b8716529728da1c8
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08546391B2

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