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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Benzyl mercaptan → HCID 57523125, 화합물

HRID 79013
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HRID 79013 반응식
CC(C)([O-])C.[K+].[CH2:7]([SH:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[C:15]([O:19][C:20](=[O:31])[C:21]1[CH:26]=[CH:25][C:24]([CH:27]=[O:28])=[C:23](F)[C:22]=1[F:30])([CH3:18])([CH3:17])[CH3:16]>C1COCC1>[C:15]([O:19][C:20](=[O:31])[C:21]1[CH:26]=[CH:25][C:24]([CH:27]=[O:28])=[C:23]([S:14][CH2:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:22]=1[F:30])([CH3:18])([CH3:16])[CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7509Benzyl mercaptanHCID 23665647Potassium tert-butoxideHCID 57523124HCID 57523124, 화합물

생성물 1

HCID 57523125HCID 57523125, 화합물수율 100%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a solution of potassium tert-butoxide (2.0 g, 17.9 mmol) in anhydrous THF (80 mL) was added benzyl mercaptan (2.1 mL, 17.9 mmol). The reaction mixture was stirred at room temperature for 5 minutes before being cooled to −30° C. A solution of 2,3-difluoro-4-formyl-benzoic acid tert-butyl ester (4.34 g, 17.9 mmol) in anhydrous THF (20 mL) was added dropwise over 15 minutes and the resultant mixture was stirred at −30° C. for 30 minutes before being quenched by addition of water and extracted with ethyl acetate. The organic layer was separated, washed with water followed by brine, dried (Na2SO4), filtered and evaporated in vacuo to give the title compound as a yellow oil (6.2 g, 100%). 1H NMR (CDCl3, 400 MHz) 10.20 (1 H, d, J=0.6 Hz), 7.84 (1 H, ddd, J=8.0, 6.8, 0.7 Hz), 7.59 (1 H, dd, J=8.0, 0.9 Hz), 7.19 (3 H, m), 7.05 (2 H, m), 4.07 (2 H, s), 1.63 (9 H, s).

후처리

  1. temperaturebefore being cooled to −30° C
  2. custombefore being quenched by addition of water
  3. extractionextracted with ethyl acetate
  4. customThe organic layer was separated
  5. washwashed with water
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-6d36d1b4f9914ec4a7056c583b6151a3
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08841462B2

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