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Diisopropylethylamine → HCID 86672807, 화합물

HRID 1755136
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HRID 1755136 반응식
[CH2:1]([O:5][C:6]1[CH:7]=[C:8]([C:16]2[NH:20][C:19](=[O:21])[C:18]3([CH2:26][CH2:25][N:24]([S:27]([CH2:30][CH2:31][C:32]4[CH:40]=[CH:39][C:35]([C:36]([OH:38])=O)=[CH:34][C:33]=4[CH3:41])(=[O:29])=[O:28])[CH2:23][CH2:22]3)[N:17]=2)[CH:9]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:11]=1)[CH2:2][C:3]#[CH:4].Cl.[N:43]([CH2:46][CH2:47][CH2:48][NH:49][CH3:50])=[N+:44]=[N-:45].CCN(C(C)C)C(C)C.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>CN(C=O)C.C(OCC)(=O)C>[N:43]([CH2:46][CH2:47][CH2:48][N:49]([CH3:50])[C:36](=[O:38])[C:35]1[CH:39]=[CH:40][C:32]([CH2:31][CH2:30][S:27]([N:24]2[CH2:23][CH2:22][C:18]3([N:17]=[C:16]([C:8]4[CH:9]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:11]=[C:6]([O:5][CH2:1][CH2:2][C:3]#[CH:4])[CH:7]=4)[NH:20][C:19]3=[O:21])[CH2:26][CH2:25]2)(=[O:28])=[O:29])=[C:33]([CH3:41])[CH:34]=1)=[N+:44]=[N-:45]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 86672806HCID 86672806, 화합물HCID 86672808(3-Azidopropyl)(methyl)amine hydrochloride

생성물 1

HCID 86672807HCID 86672807, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

4-{2-[2-(3-But-3-ynyloxy-5-trifluoromethyl-phenyl)-4-oxo-1,3,8-triaza-spiro[4.5]dec-1-ene-8-sulfonyl]-ethyl}-3-methyl-benzoic acid, (3-azido-propyl)-methyl-amine hydrochloride (15.3 mg, 0.101 mmol) and DIPEA (0.044 ml, 0.255 mmol) were dissolved in DMF (0.400 ml). HATU (0.038 mg, 0.101 mmol) was added and the mixture was stirred at room temperature for one hour. The reaction solution was diluted with ethyl acetate, and the organic layer was then washed with a 1 M aqueous hydrochloric acid solution, an aqueous sodium bicarbonate solution and saline. The organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The resulting residue was purified by column chromatography (dichloromethane-ethyl acetate) to give N-(3-azido-propyl)-4-{2-[2-(3-but-3-ynyloxy-5-trifluoromethyl-phenyl)-4-oxo-1,3,8-triaza-spiro[4.5]dec-1-ene-8-sulfonyl]-ethyl}-3,N-dimethyl-benzamide as a colorless oily substance.

후처리

  1. washthe organic layer was then washed with a 1 M aqueous hydrochloric acid solution
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe resulting residue was purified by column chromatography (dichloromethane-ethyl acetate)

출처 및 근거

ORD 기록
ord-c9ba09b9f9c94233ab79eb64e67de4ec
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09169254B2

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