Hydrochloric Acid → Ethyl 4-amino-4-(2-ethoxy-6-fluorophenyl)-2-methylbutanoate

HRID 594358

反応式

HRID 594358 の反応式
CC(C)(S([NH:6][CH:7]([C:16]1[C:21]([F:22])=[CH:20][CH:19]=[CH:18][C:17]=1[O:23][CH2:24][CH3:25])[CH2:8][CH:9]([CH3:15])[C:10]([O:12][CH2:13][CH3:14])=[O:11])=O)C.Cl.O1CCOCC1>CCO>[NH2:6][CH:7]([C:16]1[C:21]([F:22])=[CH:20][CH:19]=[CH:18][C:17]=1[O:23][CH2:24][CH3:25])[CH2:8][CH:9]([CH3:15])[C:10]([O:12][CH2:13][CH3:14])=[O:11]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 86695628Ethyl 4-(1,1-dimethylethylsulfinamido)-4-(2-ethoxy-6-fluorophenyl)-2-methylbutanoate

生成物 1

HCID 69083532Ethyl 4-amino-4-(2-ethoxy-6-fluorophenyl)-2-methylbutanoate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

A cooled (0° C.) solution of ethyl 4-(1,1-dimethylethylsulfinamido)-4-(2-ethoxy-6-fluorophenyl)-2-methylbutanoate (1.550 g; 4.00 mmol) in EtOH (20 ml) was treated dropwise with a solution of 4 M HCl in 1,4-dioxane (2.0 ml; 8.00 mmol). The resulting mixture was further stirred at 0° C., under nitrogen, for 10 min., and then at rt for 30 min. The reaction mixture was then concentrated to dryness under reduced pressure and the oily residue was further dried under HV to give the chlorhydrate salt of ethyl 4-amino-4-(2-ethoxy-6-fluorophenyl)-2-methylbutanoate. LC-MS (conditions A): tR=0.55 min. and [M+H]+: 284.07 g/mol; tR=0.57 min. and [M+H]+: 284.07 g/mol (mixture of diastereoisomers).

後処理

  1. waitat rt for 30 min
  2. concentrationThe reaction mixture was then concentrated to dryness under reduced pressure
  3. customthe oily residue was further dried under HV

出典と根拠

ORDレコード
ord-6df2a8f044bb4c0fbd2c67069f1fa547
出典データセット
uspto-grants-2016_01
特許番号
US09242970B2

関連ノート

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