Hydrochloric Acid → 4-Chloro-2-methylsulphonyl-3-(2,2,2-trifluoroethoxy)benzoic acid

HRID 2256975노트

반응식

HRID 2256975 반응식
[H-].[Na+].[F:3][C:4]([F:8])([F:7])[CH2:5][OH:6].[Cl:9][C:10]1[CH:18]=[CH:17][C:13]([C:14]([OH:16])=[O:15])=[C:12]([S:19]([CH3:22])(=[O:21])=[O:20])[C:11]=1F.Cl>C1COCC1>[Cl:9][C:10]1[CH:18]=[CH:17][C:13]([C:14]([OH:16])=[O:15])=[C:12]([S:19]([CH3:22])(=[O:21])=[O:20])[C:11]=1[O:6][CH2:5][C:4]([F:8])([F:7])[F:3]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 64092,2,2-TrifluoroethanolHCID 24758Sodium hydrideHCID 544424304-Chloro-3-fluoro-2-methylsulphonylbenzoic acid

생성물 1

HCID 545681774-Chloro-2-methylsulphonyl-3-(2,2,2-trifluoroethoxy)benzoic acid수율 99.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

Sodium hydride (1.05 g of 80% powder) was suspended in THF and to this was added a solution of 2,2,2-trifluoroethanol (1.9 g) in THF, followed by a solution of 4-chloro-3-fluoro-2-methylsulphonylbenzoic acid (4 g) in THF. The resultant mixture was stirred for 2 hours and then acidified with 2 M HCl. The mixture was extracted with ether, washed with water, dried (anhydrous magnesium sulphate) and filtered. The filtrate was evaporated to dryness yielding 4-chloro-2-methylsulphonyl-3-(2,2,2-trifluoroethoxy)benzoic acid (5.26 g) as a whim solid, NMR (DMSO d6) 2.5(s,3H), 4.8(q,2H), 7.5(d,1H), 8.0(d,1H).

후처리

  1. extractionThe mixture was extracted with ether
  2. washwashed with water
  3. dry with materialdried (anhydrous magnesium sulphate)
  4. filtrationfiltered
  5. customThe filtrate was evaporated to dryness

출처 및 근거

ORD 기록
ord-a591640f1ff94b7fa07fc945dcc3bdae
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05656573

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