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L-Pyroglutamic Acid → (S)-2-benzylcarbamoyl-5-oxo-pyrrolidine-1-carboxylic acid tert-butyl ester

HRID 925520
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반응식

HRID 925520 반응식
C1(N=C=NC2CCCCC2)CCCCC1.[NH:16]1[C:20](=[O:21])[CH2:19][CH2:18][C@H:17]1[C:22]([OH:24])=O.[CH2:25]([NH2:32])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.[C:33](OC([O-])=O)([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34].C(N(CC)CC)C>CN(C)C=O.CN(C)C1C=CN=CC=1>[C:36]([O:35][C:33]([N:16]1[C:20](=[O:21])[CH2:19][CH2:18][C@H:17]1[C:22](=[O:24])[NH:32][CH2:25][C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)=[O:34])([CH3:39])([CH3:38])[CH3:37]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 7405L-Pyroglutamic AcidHCID 7504BenzylamineHCID 8471TriethylamineHCID 10868DicyclohexylcarbodiimideHCID 22064466Tert-butyldicarbonate

생성물 1

HCID 71114834(S)-2-benzylcarbamoyl-5-oxo-pyrrolidine-1-carboxylic acid tert-butyl ester수율 17.5%

시약·촉매·용매

2
HCID 142844-(Dimethylamino)pyridine촉매HCID 6228Dimethylformamide용매

실험 절차

N,N′-Dicyclohexyl carbodiimide (DCC; 8.2 g, 40 mmol) was added to a solution of pyroglutamic acid (5.16 g, 40 mmol) in dimethylformamide (DMF; 60 ml). The mixture was stirred at room temperature for 2 h and a precipitate formed. Benzylamine (4.8 ml, 44 mmol) was added and the mixture was stirred for 2 h. t-butyl dicarbonate (Boc2O; 9.6 g, 44 mmol), triethylamine (TEA; 6.3 ml, 44 mmol) and 4-dimethylaminopyridine (DMAP; 488 mg, 4 mmol) were added and the mixture was stirred at room temperature for 16 h. The DMF was removed under vacuum and the residue was taken up with water (20 ml) and extracted with dichloromethane (DCM; 3×20 ml). The organic layers were concentrated and the crude product was purified via silica gel chromatography to afford (S)-2-benzylcarbamoyl-5-oxo-pyrrolidine-1-carboxylic acid tert-butyl ester (2.23 g, 7.0 mmol, 17.5%).

후처리

  1. customa precipitate formed
  2. additionwere added
  3. stirringthe mixture was stirred at room temperature for 16 h
  4. customThe DMF was removed under vacuum
  5. extractionextracted with dichloromethane (DCM; 3×20 ml)
  6. concentrationThe organic layers were concentrated
  7. customthe crude product was purified via silica gel chromatography

출처 및 근거

ORD 기록
ord-da7dfedd21d84dcbaca15262f10fdc77
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09284314B2

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