Diethyl Pyrocarbonate → HCID 10768458, 화합물

HRID 1720799노트

반응식

HRID 1720799 반응식
[CH2:1]([O:8][C:9]([NH:11][CH2:12][C:13]1[CH:21]=[CH:20][C:16]([C:17]([OH:19])=O)=[CH:15][CH:14]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[C:23]([O:27][C:28](=[O:40])[C@H:29]([CH2:31][CH2:32][C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34])[NH2:30])([CH3:26])([CH3:25])[CH3:24].CCOC(OC(OCC)=O)=O.C(N(CC)CC)C>CN(C)C=O>[C:23]([O:27][C:28](=[O:40])[C@H:29]([CH2:31][CH2:32][C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34])[NH:30][C:17](=[O:19])[C:16]1[CH:15]=[CH:14][C:13]([CH2:12][NH:11][C:9]([O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[O:10])=[CH:21][CH:20]=1)([CH3:25])([CH3:26])[CH3:24]

참가 물질

6

반응물 4

HCID 3051Diethyl PyrocarbonateHCID 8471TriethylamineHCID 208636Di-tert-butyl glutamate hydrochlorideHCID 14799974-((((Benzyloxy)carbonyl)amino)methyl)benzoic acid

생성물 1

HCID 10768458HCID 10768458, 화합물수율 100%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 4-(benzyloxycarbonylaminomethyl)benzoic acid as obtained in Reference Example 35 (1.0 g), glutamic acid di-t-butyl ester hydrochloride (1.15 g) and DEPC (860 mg) in dimethylformamide (20 ml), triethylamine (1.06 g) was added drop by drop, followed by stirring at room temperature for 1 hour. After solvent concentration under reduced pressure, the resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1) to yield the title compound (1.86 g, yield 100%) as a colorless wax-like substance.

후처리

  1. additionwas added drop by drop
  2. concentrationAfter solvent concentration under reduced pressure
  3. customthe resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=2:1)

출처 및 근거

ORD 기록
ord-7e4da600b05d4c14bdc78ee3eef87aa7
출처 데이터셋
uspto-grants-1996_04
특허 번호
US05506267

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