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Dichloromethane → HCID 136377183, 화합물

HRID 1027303
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HRID 1027303 반응식
Cl[C:2]1[N:7]=[N:6][C:5]([N:8]2[CH2:12][C@@H:11]3[CH2:13][N:14]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:15][C@@H:10]3[CH2:9]2)=[CH:4][CH:3]=1.[Cl:23][C:24]1[CH:25]=[CH:26][C:27](B2OC(C)(C)C(C)(C)O2)=[C:28]([OH:30])[CH:29]=1.C(=O)([O-])[O-].[Na+].[Na+].C(Cl)Cl>O1CCOCC1.O.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[Cl:23][C:24]1[CH:25]=[CH:26][C:27]([C:2]2[N:7]=[N:6][C:5]([N:8]3[CH2:12][C@@H:11]4[CH2:13][N:14]([C:16]([O:18][C:19]([CH3:21])([CH3:20])[CH3:22])=[O:17])[CH2:15][C@@H:10]4[CH2:9]3)=[CH:4][CH:3]=2)=[C:28]([OH:30])[CH:29]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 6344DichloromethaneHCID 10340Sodium CarbonateHCID 44190436HCID 44190436, 화합물HCID 676093145-Chloro-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenol

생성물 1

HCID 136377183HCID 136377183, 화합물수율 43.2%

시약·촉매·용매 3

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
촉매
HCID 962Water용매
HCID 312751,4-Dioxane용매

반응 조건

온도
90 °C

실험 절차

The reaction mixture of (3aR,6aS)-tert-butyl 5-(6-chloropyridazin-3-yl)hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate (325 mg, 1 mmol), 5-chloro-2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)phenol (280 mg, 1.100 mmol), sodium carbonate (318 mg, 3.00 mmol) and PdCl2(dppf).CH2Cl2 (61.2 mg, 0.075 mmol) in dioxane (5 mL) and water (5.00 mL) was degassed by bubbling N2 for 10 minutes. After heating at 90° C. overnight, the reaction mixture was filtered through celite and washed with EtOAc. The filtrate was concentrated and the residue was purified by silica gel chromatography (0-10% MeOH/DCM) to afford (3aR,6aS)-tert-butyl 5-(6-(4-chloro-2-hydroxyphenyl)pyridazin-3-yl)hexahydropyrrolo[3,4-c]pyrrole-2(1H)-carboxylate (180 mg, 0.432 mmol, 43.2% yield) MS (M+1)=417.0.

후처리

  1. customby bubbling N2 for 10 minutes
  2. filtrationthe reaction mixture was filtered through celite
  3. washwashed with EtOAc
  4. concentrationThe filtrate was concentrated
  5. customthe residue was purified by silica gel chromatography (0-10% MeOH/DCM)

출처 및 근거

ORD 기록
ord-03cd43980b7c4a67b0e6a073d070a908
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08729263B2

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