Hydrochloric Acid → ((2S)-2-amino-3-methylbutyl)carbamic acid p-nitrobenzyl ester hydrochloride

HRID 891766ノート

反応式

HRID 891766 の反応式
[N+:1]([C:4]1[CH:27]=[CH:26][C:7]([CH2:8][O:9][C:10](=[O:25])[NH:11][CH2:12][C@@H:13]([NH:17]C(OC(C)(C)C)=O)[CH:14]([CH3:16])[CH3:15])=[CH:6][CH:5]=1)([O-:3])=[O:2].[ClH:28]>O1CCOCC1>[ClH:28].[N+:1]([C:4]1[CH:27]=[CH:26][C:7]([CH2:8][O:9][C:10](=[O:25])[NH:11][CH2:12][C@@H:13]([NH2:17])[CH:14]([CH3:15])[CH3:16])=[CH:6][CH:5]=1)([O-:3])=[O:2]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 69544030((2S)-2-t-butoxycarbonylamino-3-methylbutyl)carbamic acid p-nitrobenzyl ester

生成物 1

HCID 69544240((2S)-2-amino-3-methylbutyl)carbamic acid p-nitrobenzyl ester hydrochloride収率 70%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

To a solution of ((2S)-2-t-butoxycarbonylamino-3-methylbutyl)-carbamic acid p-nitrobenzyl ester (3.13 g, 8.21 mmol) (obtained as described in Reference Example 61(3)) in 1,4-dioxane (31 ml) was added a 4N solution of hydrogen chloride in 1,4-dioxane (31 ml) in an ice bath, and the mixture was stirred at room temperature for 4 hours. After checking the completion of the reaction, the reaction mixture was concentrated under reduced pressure. Ethyl acetate was added to the residue, and the resulting mixture was filtered off and washed with ethyl acetate to give ((2S)-2-amino-3-methylbutyl)carbamic acid p-nitrobenzyl ester hydrochloride (1.82 g, yield 70%) as pale yellow crystals.

後処理

  1. customthe completion of the reaction
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. additionEthyl acetate was added to the residue
  4. filtrationthe resulting mixture was filtered off
  5. washwashed with ethyl acetate

出典と根拠

ORDレコード
ord-58203e05c0824c04a2f5576a5da5ae0f
出典データセット
uspto-grants-2006_02
特許番号
US07001897B2

反応ノート

読み込み中…