Lithium hydroxide, monohydrate → HCID 68328073, 화합물

HRID 2274901노트

반응식

HRID 2274901 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:9][CH:10]=[C:11]([C:13]([CH3:20])([CH3:19])[C:14]([O:16]CC)=[O:15])[N:12]=2)=[CH:4][CH:3]=1.O.[OH-].[Li+]>C1COCC1.C(O)C.O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[S:9][CH:10]=[C:11]([C:13]([CH3:20])([CH3:19])[C:14]([OH:16])=[O:15])[N:12]=2)=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 68327815HCID 68327815, 화합물

생성물 1

HCID 68328073HCID 68328073, 화합물수율 98.2%

시약·촉매·용매 1

HCID 18504229Ethanol tetrahydrofuran water용매

실험 절차

To a stirred solution of ethyl 2-(2-(4-fluorophenyl)thiazol-4-yl)-2-methylpropanoate (4.56 g, 15.5 mmol) in 1:1:1 THF/ethanol/water (45 mL) was added lithium hydroxide monohydrate (2.93 g, 69.8 mmol). The reaction was stirred overnight, concentrated and redissolved in water (175 mL). The solution was washed with ether (1×100 mL), acidified by the addition of 1.0 N HCl (80 mL) and extracted with ethyl acetate (2×70 mL). The combined extracts were dried (Na2SO4) and concentrated to afford 2-(2(4-fluorophenyl)thiazol-4-yl)-2-methylpropanoic acid as a white solid (4.04 g, 98%). This material was used in the next step without purification.

후처리

  1. concentrationconcentrated
  2. dissolutionredissolved in water (175 mL)
  3. washThe solution was washed with ether (1×100 mL)
  4. additionacidified by the addition of 1.0 N HCl (80 mL)
  5. extractionextracted with ethyl acetate (2×70 mL)
  6. dry with materialThe combined extracts were dried (Na2SO4)
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e8b6cec4c5cc4d7eab74caa56859b65f
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09126993B2

반응 노트

불러오는 중…