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

HRID 1584572ノート

反応式

HRID 1584572 の反応式
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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b814c23aab444e8c9962a29cf0daa8ca
出典データセット
uspto-grants-1999_08
特許番号
US05932733

反応ノート

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