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Cesium carbonate → HCID 42629727, 화합물

HRID 1880615
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HRID 1880615 반응식
[N:1]1([C:7]2[C:12](/[CH:13]=[CH:14]/[C:15](O)=[O:16])=[CH:11][CH:10]=[C:9]([C:18]([F:21])([F:20])[F:19])[N:8]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(=O)([O-])[O-].[Cs+].[Cs+].Br.[Cl:29][C:30]1[C:39]([OH:40])=[C:38]([OH:41])[C:37]([Cl:42])=[C:36]2[C:31]=1[CH2:32][CH2:33][NH:34][CH2:35]2.CCN=C=NCCCN(C)C.Cl.C1C=CC2N(O)N=NC=2C=1>C1COCC1.CN(C1C=CN=CC=1)C.O>[Cl:29][C:30]1[C:39]([OH:40])=[C:38]([OH:41])[C:37]([Cl:42])=[C:36]2[C:31]=1[CH2:32][CH2:33][N:34]([C:15](=[O:16])/[CH:14]=[CH:13]/[C:12]1[C:7]([N:1]3[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]3)=[N:8][C:9]([C:18]([F:21])([F:20])[F:19])=[CH:10][CH:11]=1)[CH2:35]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 5

HCID 10796Cesium carbonateHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 59830359HCID 59830359, 화합물HCID 685081725,8-Dichloro-1,2,3,4-tetrahydroisoquinoline-6,7-diol hydrobromide

생성물 1

HCID 42629727
HCID 42629727, 화합물
수율 24%

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

(E)-3-(2-(piperidin-1-yl)-6-(trifluoromethyl)pyridin-3-yl)acrylic acid (150.0 mg, 0.50 mmol) was suspended in dry THF (7.0 mL). DMAP (111.4 mg, 0.91 mmol) and caesium carbonate (296.0 mg, 0.91 mmol) were added and the mixture was stirred at rt for 15 minutes. 5,8-Dichloro-6,7-dihydroxy-1,2,3,4-tetrahydroisoquinoline hydrobromide (143.0 mg, 0.45 mmol), EDC.HCl (130.6 mg, 0.68 mmol), HOBt (69.8 mg, 0.45 mmol) were then added. The mixture was stirred at rt overnight. Water (100 mL) was added and the product extracted with EtOAc. Combined organic extracts were dried (MgSO4), filtered and concentrated. Purification was done first using flash column chromatography (CH2Cl2/MeOH 98/2→95/5) and then by size exclusion (Sephadex LH20; CHCl3/MeOH 1/1) to yield 55.0 mg (24%) of the title product.

후처리

  1. stirringThe mixture was stirred at rt overnight
  2. extractionthe product extracted with EtOAc
  3. dry with materialCombined organic extracts were dried (MgSO4)
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customPurification

출처 및 근거

ORD 기록
ord-a3d0ff963d8c42e6b5cedb6d58ebf1af
출처 데이터셋
uspto-grants-2012_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08318768B2

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