Diisopropylethylamine → 5-{9-[3-(2,5-Dioxo-pyrrolidin-1-yloxycarbonyl)-propylcarbamoyl]-nonyloxy}-isophthalic acid di-tert-butyl ester

HRID 1022422노트

반응식

HRID 1022422 반응식
[C:1]([O:5][C:6](=[O:39])[C:7]1[CH:19]=[C:18]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][C:30](=[O:38])[NH:31][CH2:32][CH2:33][CH2:34][C:35]([OH:37])=[O:36])[CH:17]=[C:9]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH:8]=1)([CH3:4])([CH3:3])[CH3:2].CCN(C(C)C)C(C)C.[B-](F)(F)(F)F.CN(C(O[N:62]1[C:67](=[O:68])[CH2:66][CH2:65][C:63]1=[O:64])=[N+](C)C)C>C1COCC1>[C:1]([O:5][C:6](=[O:39])[C:7]1[CH:19]=[C:18]([O:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][C:30](=[O:38])[NH:31][CH2:32][CH2:33][CH2:34][C:35]([O:37][N:62]2[C:67](=[O:68])[CH2:66][CH2:65][C:63]2=[O:64])=[O:36])[CH:17]=[C:9]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH:8]=1)([CH3:2])([CH3:3])[CH3:4]

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 98575222-(2,5-Dioxopyrrolidin-1-yl)-1,1,3,3-tetramethylisouronium tetrafluoroborateHCID 684424855-[9-(3-Carboxy-propylcarbamoyl)-nonyloxy]-isophthalic Acid Di-tert-butyl Ester

생성물 1

HCID 874559705-{9-[3-(2,5-Dioxo-pyrrolidin-1-yloxycarbonyl)-propylcarbamoyl]-nonyloxy}-isophthalic acid di-tert-butyl ester

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 5-[9-(3-Carboxy-propylcarbamoyl)-nonyloxy]-isophthalic acid di-tert-butyl ester (62 mg, 0.11 mmol) in dry THF (2 ml) was added DIPEA (0.05 ml) and TSTU (41 mg, 0.14 mmol). The mixture was stirred at room temperature under nitrogen over night. The mixture was concentrated and EtOAc was added to the residue. The precipitate was removed by filtration. The filtrate was washed with 0.1 N HCl (2×) and brine (1×), dried (Na2SO4) and concentrated to give a clear syrup.

후처리

  1. concentrationThe mixture was concentrated
  2. additionEtOAc was added to the residue
  3. customThe precipitate was removed by filtration
  4. washThe filtrate was washed with 0.1 N HCl (2×) and brine (1×)
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated
  7. customto give a clear syrup

출처 및 근거

ORD 기록
ord-c8b64bf5562849d58bef4b39a1abe703
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722620B2

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