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

HRID 891766노트

반응식

HRID 891766 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-58203e05c0824c04a2f5576a5da5ae0f
출처 데이터셋
uspto-grants-2006_02
특허 번호
US07001897B2

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