Hydrochloric Acid → Methyl 4-amino-4-(2,4-dimethoxypyridin-3-yl)-2-methylbutanoate

HRID 594362ノート

反応式

HRID 594362 の反応式
[CH3:1][O:2][C:3]1[C:8]([CH:9]([NH:18]S(C(C)(C)C)=O)[CH2:10][CH:11]([CH3:17])[C:12]([O:14][CH2:15]C)=[O:13])=[C:7]([O:25][CH3:26])[CH:6]=[CH:5][N:4]=1.Cl.O1CCOCC1>CO>[NH2:18][CH:9]([C:8]1[C:3]([O:2][CH3:1])=[N:4][CH:5]=[CH:6][C:7]=1[O:25][CH3:26])[CH2:10][CH:11]([CH3:17])[C:12]([O:14][CH3:15])=[O:13]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 69082487Ethyl 4-(2,4-dimethoxypyridin-3-yl)-4-(1,1-dimethylethylsulfinamido)-2-methylbutanoate

生成物 1

HCID 69085168Methyl 4-amino-4-(2,4-dimethoxypyridin-3-yl)-2-methylbutanoate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
0 °C

実験手順

A cooled (0° C.) solution of ethyl 4-(2,4-dimethoxypyridin-3-yl)-4-(1,1-dimethylethylsulfinamido)-2-methylbutanoate (0.709 g; 1.83 mmol) in MeOH (15 ml) was treated dropwise with a solution of 4 M HCl in 1,4-dioxane (0.92 ml; 3.67 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 methyl 4-amino-4-(2,4-dimethoxypyridin-3-yl)-2-methylbutanoate. LC-MS (conditions B): tR=0.45 min. and [M+H]+: 269.33 g/mol; tR=0.47 min. and [M+H]+: 269.33 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-62ecc8d9c74c425d8f1c115510cafebe
出典データセット
uspto-grants-2016_01
特許番号
US09242970B2

反応ノート

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