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

HRID 1943091ノート

反応式

HRID 1943091 の反応式
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]

参加物

5

反応物 2

HCID 313Hydrochloric AcidHCID 444750373-sulfinylamino-N-[2-ethyl-6-methyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethyl-ethyl)-phenyl]-benzamide

生成物 1

HCID 441994443-amino-N-[2-ethyl-6-methyl-4-(1,2,2,2-tetrafluoro-1-trifluoromethyl-ethyl)-phenyl]-benzamide

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5b869890caab407eb2019df508d11e34
出典データセット
uspto-grants-2013_03
特許番号
US08389767B2

反応ノート

読み込み中…