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1,4-Dioxane → HCID 57377354, 화합물

HRID 72555
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HRID 72555 반응식
[Cl:1][C:2]1[CH:3]=[N:4][C:5]([N:24]2[CH2:28][CH2:27][CH:26]([O:29][C:30]3[CH:35]=[CH:34][C:33]([C:36]([F:39])([F:38])[F:37])=[CH:32][CH:31]=3)[CH2:25]2)=[C:6]([CH:23]=1)[C:7]([NH:9][C:10]1([C:13]2[CH:22]=[CH:21][C:16]([C:17]([O:19]C)=[O:18])=[CH:15][CH:14]=2)[CH2:12][CH2:11]1)=[O:8].O1CCOCC1.O.[OH-].[Li+]>O>[Cl:1][C:2]1[CH:3]=[N:4][C:5]([N:24]2[CH2:28][CH2:27][CH:26]([O:29][C:30]3[CH:31]=[CH:32][C:33]([C:36]([F:37])([F:39])[F:38])=[CH:34][CH:35]=3)[CH2:25]2)=[C:6]([CH:23]=1)[C:7]([NH:9][C:10]1([C:13]2[CH:14]=[CH:15][C:16]([C:17]([OH:19])=[O:18])=[CH:21][CH:22]=2)[CH2:12][CH2:11]1)=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 312751,4-DioxaneHCID 168937Lithium hydroxide, monohydrateHCID 67958319HCID 67958319, 화합물

생성물 1

HCID 57377354HCID 57377354, 화합물수율 6.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of methyl 4-(1-(5-chloro-2-(3-(4-(trifluoromethyl)phenoxy)pyrrolidin-1-yl)nicotinamido)cyclopropyl)benzoate (D199) (24 mg, 0.428 mmol) in a mixture 1,4-dioxane and water (3 ml/1 ml) lithium hydroxide monohydrate (2.7 mg, 0.064 mmol) was added and the mixture was stirred 2 days at room temperature. After solvent evaporation the residue was diluted with water (5 ml) and HCl 1M (15 ml) and extracted with ethylacetate (3×20 ml). Collected organics after solvent evaporation gave the title compound (E73) (15 mg) as racemic mixture.

후처리

  1. customAfter solvent evaporation the residue
  2. additionwas diluted with water (5 ml) and HCl 1M (15 ml)
  3. extractionextracted with ethylacetate (3×20 ml)
  4. customCollected organics after solvent evaporation

출처 및 근거

ORD 기록
ord-685b89d02421444e83c25d3dc76f75e9
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08828987B2

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