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Diisopropylethylamine → HCID 87218236, 화합물

HRID 593235
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HRID 593235 반응식
[O:1]=[C:2]1[CH:6]=[CH:5][C:4](=[O:7])[N:3]1[CH2:8][CH2:9][C:10]([NH:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][C:20]([OH:22])=[O:21])=[O:11].[B-](F)(F)(F)F.CN(C(O[N:36]1[C:41](=[O:42])[CH2:40][CH2:39][C:37]1=[O:38])=[N+](C)C)C.CCN(C(C)C)C(C)C>C1COCC1>[O:38]=[C:37]1[CH2:39][CH2:40][C:41](=[O:42])[N:36]1[O:21][C:20](=[O:22])[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][NH:12][C:10](=[O:11])[CH2:9][CH2:8][N:3]1[C:4](=[O:7])[CH:5]=[CH:6][C:2]1=[O:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 98575222-(2,5-Dioxopyrrolidin-1-yl)-1,1,3,3-tetramethylisouronium tetrafluoroborateHCID 66968126Octanoic acid, 8-[[3-(2,5-dihydro-2,5-dioxo-1H-pyrrol-1-yl)-1-oxopropyl]amino]-

생성물 1

HCID 87218236HCID 87218236, 화합물수율 37%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 8-[3-(2,5-dioxo-2,5-dihydropyrrol-1-yl)propionylamino]octanoic acid (917 mg, crude) in dry THF (15 ml) was added TSTU (1.07 mg) and DIPEA (0.65 ml). The mixture was stirred under nitrogen over night. The mixture was concentrated. To the residue was added EtOAc and the precipitate was filtered off. The filtrate was extracted with 0.1 N HCl (2×) and brine (1×), dried (Na2SO4) and concentrated to give an off-white solid. Overall yield 37% (444 mg). LC-MS, M/z: 408.39 (M+1).

후처리

  1. concentrationThe mixture was concentrated
  2. additionTo the residue was added EtOAc
  3. filtrationthe precipitate was filtered off
  4. extractionThe filtrate was extracted with 0.1 N HCl (2×) and brine (1×)
  5. dry with materialdried (Na2SO4)
  6. concentrationconcentrated
  7. customto give an off-white solid

출처 및 근거

ORD 기록
ord-647f5ccc58084c96951afa7f6d2c4522
출처 데이터셋
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09242011B2

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