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

HRID 73499
ノート
印刷プレビュー

反応式

HRID 73499 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

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

生成物 1

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

試薬・触媒・溶媒

2
HCID 142844-(Dimethylamino)pyridine触媒HCID 6228Dimethylformamide溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-c29b893a97a54d9590df659b272e770b
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08829191B2

反応ノート

読み込み中…

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