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4-Methoxybenzaldehyde → HCID 11490484、化合物

HRID 1727039
ノート
印刷プレビュー

反応式

HRID 1727039 の反応式
[NH2:1][CH2:2][CH2:3][N:4]1[C:8]2=[N:9][C:10]([N:13]([CH2:19][CH2:20][CH:21]([CH3:23])[CH3:22])[CH2:14][CH2:15][CH:16]([CH3:18])[CH3:17])=[CH:11][CH:12]=[C:7]2[N:6]=[C:5]1[NH:24][C:25]1[CH:30]=[C:29]([O:31][CH3:32])[C:28]([O:33][CH3:34])=[C:27]([O:35][CH3:36])[CH:26]=1.[CH:37](=O)[C:38]1[CH:43]=[CH:42][C:41]([O:44][CH3:45])=[CH:40][CH:39]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].C(=O)([O-])O.[Na+]>ClCCl.CO.O>[CH3:45][O:44][C:41]1[CH:42]=[CH:43][C:38]([CH2:37][NH:1][CH2:2][CH2:3][N:4]2[C:8]3=[N:9][C:10]([N:13]([CH2:14][CH2:15][CH:16]([CH3:18])[CH3:17])[CH2:19][CH2:20][CH:21]([CH3:22])[CH3:23])=[CH:11][CH:12]=[C:7]3[N:6]=[C:5]2[NH:24][C:25]2[CH:30]=[C:29]([O:31][CH3:32])[C:28]([O:33][CH3:34])=[C:27]([O:35][CH3:36])[CH:26]=2)=[CH:39][CH:40]=1
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 4

HCID 312444-MethoxybenzaldehydeHCID 516892Sodium BicarbonateHCID 5049666Sodium triacetoxyborohydrideHCID 57566331HCID 57566331、化合物

生成物 1

HCID 11490484HCID 11490484、化合物収率 68%

試薬・触媒・溶媒 3

HCID 887Methanol
溶媒
HCID 962Water溶媒
HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 3-(2-aminoethyl)-N5,N5-bis(3-methylbutyl)-N2-(3,4,5-trimethoxyphenyl)-3H-imidazo[4,5-b]pyridine-2,5-diamine (83 mg, 1 eq) and p-anisaldehyde (25 mg, 1 eq) in dichloromethane (1.5 ml) is stirred for 6 hours at a temperature of approximately 20° C. The mixture is diluted with methanol (2 ml) then sodium triacetoxyborohydride (70 mg, 2 eq) is added. After stirring for 0.5 hour at a temperature of approximately 20° C., dichloromethane (20 ml) and water saturated with sodium hydrogen carbonate (10 ml) are added to the mixture. After decantation and extractions, the combined organic phases are washed with salt water, dried over Na2SO4 then concentrated under reduced pressure at 40° C. Purification of the residue by flash chromatography on silica gel (eluent: heptane/ethyl acetate 1:1 to 2:8) produces the expected compound (70 mg, 68% yield).

後処理

  1. additionare added to the mixture
  2. extractionAfter decantation and extractions
  3. washthe combined organic phases are washed with salt water
  4. dry with materialdried over Na2SO4
  5. concentrationthen concentrated under reduced pressure at 40° C
  6. customPurification of the residue by flash chromatography on silica gel (eluent: heptane/ethyl acetate 1:1 to 2:8)

出典と根拠

ORDレコード
ord-02defa71186e4b1ca94d0a46f10bd066
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07495009B2

反応ノート

読み込み中…

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