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N-(tert-butoxycarbonyl)glycine → HCID 18475838, 화합물

HRID 2187876
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HRID 2187876 반응식
[C:1]([O:5][C:6]([NH:8][CH2:9][C:10]([OH:12])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].C1CN([P+](ON2N=NC3C=CC=CC2=3)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.[NH2:46][C:47]1[C:56]2[C:51](=[CH:52][CH:53]=[C:54]([O:57][CH2:58][C:59]3[CH:64]=[CH:63][CH:62]=[CH:61][CH:60]=3)[CH:55]=2)[CH:50]=[CH:49][CH:48]=1.C(N(CC)C(C)C)(C)C>C(Cl)Cl>[CH2:58]([O:57][C:54]1[CH:55]=[C:56]2[C:51]([CH:50]=[CH:49][CH:48]=[C:47]2[NH:46][C:10](=[O:12])[CH2:9][NH:8][C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])=[CH:52][CH:53]=1)[C:59]1[CH:60]=[CH:61][CH:62]=[CH:63][CH:64]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 78288N-(tert-butoxycarbonyl)glycineHCID 81531DiisopropylethylamineHCID 2724699PyBOPHCID 18433613HCID 18433613, 화합물

생성물 1

HCID 18475838HCID 18475838, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To N-(tert-butoxycarbonyl)glycine (527 mg, 3.01 mmol) in dry CH2Cl2 (5 mL) under argon were added PYBOP (1.65 g, 3.16 mmol), 1-amino-7-benzyloxynaphthalene, as described above in Step J, (750 mg, 3.01 mmol), and N,N-diisopropylethylamine (0.55 mL, 3.16 mmol). The reaction mixture was stirred for 18 hrs, then partitioned between CH2Cl2 (200 mL) and 10% aqueous citric acid (50 mL). The organic layer was dried over Na2SO4, filtered, and concentrated in vacuo. The crude product was sufficiently pure for use in the next reaction.

후처리

  1. custompartitioned between CH2Cl2 (200 mL) and 10% aqueous citric acid (50 mL)
  2. dry with materialThe organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo
  5. customThe crude product was sufficiently pure for use in the next reaction

출처 및 근거

ORD 기록
ord-7d95aa5840c64f4eb17a969732875b00
출처 데이터셋
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06410534B1

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