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Sodium Hydroxide → HCID 68471024、化合物

HRID 506817
ノート
印刷プレビュー

反応式

HRID 506817 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 14798Sodium HydroxideHCID 5003444Sodium cyanoborohydrideHCID 178486707HCID 178486707、化合物

生成物 1

HCID 68471024HCID 68471024、化合物収率 46.8%

試薬・触媒・溶媒 4

HCID 3007855Zincchloride触媒HCID 887Methanol溶媒
HCID 962
Water
溶媒
HCID 6344Dichloromethane溶媒

実験手順

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:

後処理

  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

出典と根拠

ORDレコード
ord-7b762409912c4d42a781f5cbb1871623
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07786114B2

反応ノート

読み込み中…

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