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 1160397노트

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HRID 1160397 반응식
[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]

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 887Methanol용매HCID 204431481,4-Dioxane hydrochloride용매

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온도
60 °C

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-9cfef89d7617450e80e24c73c4cdc4ed
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07816395B2

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