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

HRID 594358

반응식

HRID 594358 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
0 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-6df2a8f044bb4c0fbd2c67069f1fa547
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242970B2

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