1,1-Dimethylethyl (3S)-3-[(3-chloro-4-cyanophenyl)amino]-4-(methylamino)butanoate → Methyl (3S)-3-[(3-chloro-4-cyanophenyl)amino]-4-(methylamino)butanoate, hydrochloride

HRID 1160397ノート

反応式

HRID 1160397 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:10][C@H:11]([CH2:20][NH:21][CH3:22])[CH2:12][C:13]([O:15][C:16](C)(C)C)=[O:14])[CH:5]=[CH:6][C:7]=1[C:8]#[N:9]>CO.Cl.O1CCOCC1>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([NH:10][C@H:11]([CH2:20][NH:21][CH3:22])[CH2:12][C:13]([O:15][CH3:16])=[O:14])[CH:5]=[CH:6][C:7]=1[C:8]#[N:9]

参加物

4

反応物 1

HCID 595162571,1-Dimethylethyl (3S)-3-[(3-chloro-4-cyanophenyl)amino]-4-(methylamino)butanoate

生成物 1

HCID 131728379Methyl (3S)-3-[(3-chloro-4-cyanophenyl)amino]-4-(methylamino)butanoate, hydrochloride

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 204431481,4-Dioxane hydrochloride溶媒

反応条件

温度
60 °C

実験手順

The 1,1-dimethylethyl (3S)-3-[(3-chloro-4-cyanophenyl)amino]-4-(methylamino)butanoate from the previous step (31.4 g) was dissolved in a mixture of MeOH (100 mL) and 4N HCl/dioxane (30 mL) and heated to 60° C. for 1.25 h. The solvents were concentrated to a slurry, Et2O (200 mL) was added, the solid filtered, washed well with Et2O to give the titled compound (15.6 g).

後処理

  1. concentrationThe solvents were concentrated to a slurry, Et2O (200 mL)
  2. additionwas added
  3. filtrationthe solid filtered
  4. washwashed well with Et2O

出典と根拠

ORDレコード
ord-9cfef89d7617450e80e24c73c4cdc4ed
出典データセット
uspto-grants-2010_10
特許番号
US07816395B2

反応ノート

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