1,2-Dichloroethane → HCID 58333391, 화합물

HRID 2066843노트

반응식

HRID 2066843 반응식
[CH:1]([O:4][C:5]([N:7]1[CH2:12][CH2:11][CH:10]([O:13][N:14]=[C:15]2[CH2:20][CH2:19][N:18]([C:21]3[CH:26]=[C:25]([F:27])[C:24]([CH2:28][OH:29])=[CH:23][C:22]=3[F:30])[CH2:17][CH2:16]2)[CH2:9][CH2:8]1)=[O:6])([CH3:3])[CH3:2].[C:31]([O:35][C:36]([NH:38][CH2:39][C:40](O)=[O:41])=[O:37])([CH3:34])([CH3:33])[CH3:32].C(Cl)CCl.[C+](=O)C1C=CC=CC=1>CN(C1C=CN=CC=1)C.C(Cl)Cl>[CH:1]([O:4][C:5]([N:7]1[CH2:12][CH2:11][CH:10]([O:13][N:14]=[C:15]2[CH2:16][CH2:17][N:18]([C:21]3[CH:26]=[C:25]([F:27])[C:24]([CH2:28][O:29][C:40](=[O:41])[CH2:39][NH:38][C:36]([O:35][C:31]([CH3:33])([CH3:32])[CH3:34])=[O:37])=[CH:23][C:22]=3[F:30])[CH2:19][CH2:20]2)[CH2:9][CH2:8]1)=[O:6])([CH3:3])[CH3:2]

참가 물질

7

반응물 4

HCID 111,2-DichloroethaneHCID 78288N-(tert-butoxycarbonyl)glycineHCID 5325558HCID 5325558, 화합물HCID 58333373HCID 58333373, 화합물

생성물 1

HCID 58333391HCID 58333391, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

Compound 10-1 (40 mg, 0.094 mmol), tert-butoxycarbonylamino-acetic acid (17 mg, 0.097 mmol), DMAP (3 mg, 0.024 mmol), EDC(22 mg, 0.11 mmol) and DCM (1 mL) were combined in that order and the reaction mixture was stirred for 20 h. The mixture was then washed with aqueous NaHCO3 (1 mL), concentrated under a stream of nitrogen and purified by Jones flash LC(eluent: 10-40% ethyl acetate+0.1% triethylamine in hexanes) to afford 12-1: LC-MS 408.2 (benzylium fragment).

후처리

  1. washThe mixture was then washed with aqueous NaHCO3 (1 mL)
  2. concentrationconcentrated under a stream of nitrogen
  3. custompurified by Jones flash LC(eluent
  4. custom10-40% ethyl acetate+0.1% triethylamine in hexanes) to afford 12-1

출처 및 근거

ORD 기록
ord-123b0e1df30b4c7ab70811e38c746728
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08293729B2

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