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Sodium Hydroxide → HCID 68471024, 화합물

HRID 506817
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HRID 506817 반응식
[CH3:1][O:2][C:3]1[N:8]=[C:7]2[C:9]([C:13]3[NH:30][C:16]4=[N:17][CH:18]=[CH:19][C:20](/[CH:21]=[N:22]/[C:23]5[CH:28]=[CH:27][C:26]([OH:29])=[CH:25][CH:24]=5)=[C:15]4[CH:14]=3)=[CH:10][N:11]([CH3:12])[C:6]2=[CH:5][C:4]=1[O:31][CH3:32].C([BH3-])#N.[Na+].[OH-].[Na+]>CO.O.ClCCl.[Cl-].[Zn+2].[Cl-]>[CH3:1][O:2][C:3]1[N:8]=[C:7]2[C:9]([C:13]3[NH:30][C:16]4=[N:17][CH:18]=[CH:19][C:20]([CH2:21][NH:22][C:23]5[CH:28]=[CH:27][C:26]([OH:29])=[CH:25][CH:24]=5)=[C:15]4[CH:14]=3)=[CH:10][N:11]([CH3:12])[C:6]2=[CH:5][C:4]=1[O:31][CH3:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 3

HCID 14798Sodium HydroxideHCID 5003444Sodium cyanoborohydrideHCID 178486707HCID 178486707, 화합물

생성물 1

HCID 68471024HCID 68471024, 화합물수율 46.8%

시약·촉매·용매 4

HCID 3007855Zincchloride촉매HCID 887Methanol용매
HCID 962
Water
용매
HCID 6344Dichloromethane용매

실험 절차

To a solution of 0.085 g of 4-{[1-[2-(5,6-dimethoxy-1-methyl-1H-pyrrolo[3,2-b]pyridin-3-yl)-1H-pyrrolo[2,3-b]pyridin-4-yl]meth-(E)-ylidene]amino}phenol in 20 cm3 of methanol, at a temperature in the region of 20° C., are added 0.013 g of zinc chloride and 0.013 g of sodium cyanoborohydride. The reaction medium is stirred at the same temperature for 4 hours. The reaction medium is concentrated under reduced pressure. The residue obtained is taken up in 10 cm3 of water and 25 cm3 of dichloromethane, and then basified with 0.1N sodium hydroxide. After separation of the phases by settling, the organic phase is dried over magnesium sulfate, filtered and then concentrated under reduced pressure to give 0.04 g of 4-{[2-(5,6-dimethoxy-1-methyl-1H-pyrrolo[3,2-b]pyridin-3-yl)-1H-pyrrolo[2,3-b]pyridin-4-ylmethyl]amino}phenol with the following characteristics:

후처리

  1. concentrationThe reaction medium is concentrated under reduced pressure
  2. customThe residue obtained
  3. customAfter separation of the phases
  4. dry with materialthe organic phase is dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7b762409912c4d42a781f5cbb1871623
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07786114B2

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