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Sodium Carbonate → HCID 69069158, 화합물

HRID 491150
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HRID 491150 반응식
[CH3:1]OB(O)O.C([O-])([O-])=O.[Na+].[Na+].[NH2:12][C:13]1[C:45]([Cl:46])=[CH:44][C:16]([CH2:17][C@@H:18]([CH2:23][C:24](=[O:43])[N:25]2[CH2:30][CH2:29][CH:28]([N:31]3[CH2:37][CH2:36][C:35]4[CH:38]=[CH:39][CH:40]=[CH:41][C:34]=4[NH:33][C:32]3=[O:42])[CH2:27][CH2:26]2)[C:19]([O:21][CH3:22])=[O:20])=[CH:15][C:14]=1Br>O1CCOCC1.CO.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]>[NH2:12][C:13]1[C:14]([CH3:1])=[CH:15][C:16]([CH2:17][C@@H:18]([CH2:23][C:24](=[O:43])[N:25]2[CH2:30][CH2:29][CH:28]([N:31]3[CH2:37][CH2:36][C:35]4[CH:38]=[CH:39][CH:40]=[CH:41][C:34]=4[NH:33][C:32]3=[O:42])[CH2:27][CH2:26]2)[C:19]([O:21][CH3:22])=[O:20])=[CH:44][C:45]=1[Cl:46]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 10340Sodium CarbonateHCID 14178740MethylboratHCID 69064064HCID 69064064, 화합물

생성물 1

HCID 69069158HCID 69069158, 화합물

시약·촉매·용매 3

HCID 44119782Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)촉매
HCID 887
Methanol
용매
HCID 312751,4-Dioxane용매

실험 절차

Under a nitrogen atmosphere 0.99 g (16.0 mmol) methylboric acid, 15.5 mL 2 M Na2CO3 solution and 1.02 g (1.40 mmol) Pd(dppf)Cl2 were added to a solution of 8.40 g (14.5 mmol) methyl(S)-2-(4-amino-3-bromo-5-chloro-benzyl)-4-oxo-4-[4-(2-oxo-1,2,4,5-tetrahydro-1,3-benzodiazepin-3-yl)-piperidin-1-yl]-butanoate in 50 mL 1,4-dioxane and 3 mL MeOH and the reaction mixture was refluxed overnight. The reaction solution was filtered while hot and the filtrate was combined with EtOAc. The organic phase was washed several times with semisaturated NaHCO3 solution and dried over Na2SO4. It was filtered through activated charcoal and evaporated down i.vac. The residue was taken up in a little DCM and purified by chromatography (silica gel, gradient DCM to DCM/MeOH/NH3 90:10:1). The fractions containing the product were combined, evaporated down i.vac., triturated with DIPE, suction filtered and dried.

후처리

  1. temperaturethe reaction mixture was refluxed overnight
  2. filtrationThe reaction solution was filtered while hot and the filtrate
  3. washThe organic phase was washed several times with semisaturated NaHCO3 solution
  4. dry with materialdried over Na2SO4
  5. filtrationIt was filtered through activated charcoal
  6. customevaporated down i.vac
  7. custompurified by chromatography (silica gel, gradient DCM to DCM/MeOH/NH3 90:10:1)
  8. additionThe fractions containing the product
  9. customevaporated down i.vac
  10. custom, triturated with DIPE, suction
  11. filtrationfiltered
  12. customdried

출처 및 근거

ORD 기록
ord-b929a4a669bc4c119e4d88c0df1fddac
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07528129B2

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