Hydrochloric Acid → 3-amino-N-[2-ethyl-6-methyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethyl-ethyl)-phenyl]-benzamide

HRID 1943091노트

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HRID 1943091 반응식
S(=[N:3][C:4]1[CH:5]=[C:6]([CH:29]=[CH:30][CH:31]=1)[C:7]([NH:9][C:10]1[C:15]([CH3:16])=[CH:14][C:13]([C:17]([F:26])([C:22]([F:25])([F:24])[F:23])[C:18]([F:21])([F:20])[F:19])=[CH:12][C:11]=1[CH2:27][CH3:28])=[O:8])=O.Cl>ClCCl.O1CCCC1>[NH2:3][C:4]1[CH:5]=[C:6]([CH:29]=[CH:30][CH:31]=1)[C:7]([NH:9][C:10]1[C:15]([CH3:16])=[CH:14][C:13]([C:17]([F:26])([C:22]([F:23])([F:24])[F:25])[C:18]([F:19])([F:20])[F:21])=[CH:12][C:11]=1[CH2:27][CH3:28])=[O:8]

참가 물질

5

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온도
25 °C

실험 절차

A solution of 3-sulfinylamino-N-[2-ethyl-6-methyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethyl-ethyl)-phenyl]-benzamide (0.111 g, 0.237 mmol) (for example, Example 2.1) in dichloromethane (2 ml) and tetrahydrofuran (2 ml) was treated with aqueous hydrochloric acid (2N) (1 ml) and stirred at 25° C. for 30 minutes. The organic solvents were removed from the reaction mixture under reduced pressure. The residue was neutralized with aqueous sodium hydrogen carbonate (saturated) and was extracted with dichloromethane. The organic phase was dried over sodium sulfate and evaporated to yield the desired compound. 1H-NMR (CDCl3, 400 MHz): 7.44 (s, 1H), 7.38 (s, 2H), 7.30-7.20 (m, 3H), 6.89 (d, 1H), 3.85 (bs, 2H), 2.69 (q, 2H), 2.32 (s, 3H), 1.22 (t, 3H) ppm.

후처리

  1. customThe organic solvents were removed from the reaction mixture under reduced pressure
  2. extractionwas extracted with dichloromethane
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. customevaporated

출처 및 근거

ORD 기록
ord-5b869890caab407eb2019df508d11e34
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08389767B2

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