Lithium Hydroxide → HCID 68176441, 화합물

HRID 1486967노트

반응식

HRID 1486967 반응식
[OH:1][C:2]1[CH:3]=[C:4]([C:12]2[N:16]=[CH:15][N:14](/[CH:17]=[CH:18]\[C:19]([O:21]C(C)C)=[O:20])[N:13]=2)[CH:5]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:7]=1.[Li+].[OH-]>C1COCC1.O>[OH:1][C:2]1[CH:3]=[C:4]([C:12]2[N:16]=[CH:15][N:14](/[CH:17]=[CH:18]\[C:19]([OH:21])=[O:20])[N:13]=2)[CH:5]=[C:6]([C:8]([F:9])([F:10])[F:11])[CH:7]=1

참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 53386342HCID 53386342, 화합물

생성물 1

HCID 68176441HCID 68176441, 화합물수율 85.5%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

A solution of (Z)-isopropyl 3-(3-(3-hydroxy-5-(trifluoromethyl)phenyl)-1H-1,2,4-triazol-1-yl)acrylate (4 g, 1.0 eq.) in THF (40 mL) and water (40 mL) was treated with LiOH (1.92 g, 4 eq.). The reaction mixture was stirred at RT for 2-3 hrs then quenched with acidic ice-water slurry (300 mL) and extracted with EtOAc (3×250 mL). The combined organic layers were washed with dil HCl solution (50 mL), dried over anhydrous Na2SO4 and concentrated under reduced pressure to afford 3 g of crude compound. The resulting crude off-white compound was used as such in the following step. Yield: 85.5%. Mass: (ES+) 299.92 (M+1).

후처리

  1. customthen quenched with acidic ice-water slurry (300 mL)
  2. extractionextracted with EtOAc (3×250 mL)
  3. washThe combined organic layers were washed with dil HCl solution (50 mL)
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-9d74fda233cf480288a99197613cb327
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09428490B2

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