Hydrochloric Acid → (S)-Benzyl 2-(3-amino-2-oxopiperidin-1-yl)acetate hydrochloride

HRID 1584572노트

반응식

HRID 1584572 반응식
C(OC([NH:8][C@H:9]1[CH2:14][CH2:13][CH2:12][N:11]([CH2:15][C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:17])[C:10]1=[O:26])=O)(C)(C)C.Cl.C(Cl)[Cl:29].[NH4+].[OH-]>C(OCC)(=O)C.CO>[ClH:29].[NH2:8][C@H:9]1[CH2:14][CH2:13][CH2:12][N:11]([CH2:15][C:16]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[O:17])[C:10]1=[O:26]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6344DichloromethaneHCID 14923Ammonium HydroxideHCID 10642402(S)-Benzyl 2-(3-((tert-butoxycarbonyl)amino)-2-oxopiperidin-1-YL)acetate

생성물 1

HCID 70271136(S)-Benzyl 2-(3-amino-2-oxopiperidin-1-yl)acetate hydrochloride

시약·촉매·용매 2

HCID 887Methanol용매HCID 8857Ethyl Acetate용매2회

실험 절차

To a solution of the compound of Example 38 (4.00 g, 0.0110 mole) in 10 mL of ethyl acetate at room temperature was added 5N HCl in ethyl acetate (50 mL, freshly prepared, 0.25 mole) in one portion. The solution was stirred for 3 hrs, solvent was evaporated, CH2Cl2 was added and the solvents were reevaporated. The residue was pumped at <1 mm Hg on a vacuum pump for 24 hours to afford 3.37 g (~Quantitative crude yield) of product as a colorless foam. TLC (silica gel; CH2Cl2, methanol, conc. NH4OH: 27:3:1): Rf=0.32.

후처리

  1. customfreshly prepared
  2. customsolvent was evaporated
  3. additionCH2Cl2 was added
  4. customthe solvents were reevaporated
  5. waitThe residue was pumped at <1 mm Hg on a vacuum pump for 24 hours
  6. customto afford
  7. custom3.37 g (~Quantitative crude yield) of product as a colorless foam

출처 및 근거

ORD 기록
ord-b814c23aab444e8c9962a29cf0daa8ca
출처 데이터셋
uspto-grants-1999_08
특허 번호
US05932733

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