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4-Toluenesulfonyl chloride → HCID 58833643、化合物

HRID 540869
ノート
印刷プレビュー

反応式

HRID 540869 の反応式
[CH:1]([NH:4][C:5](=[O:27])[O:6][C:7]1[CH:8]=[CH:9][C:10]2[C:11]3[N:19]([CH2:20][CH2:21][CH3:22])[C:18]([CH2:23][CH2:24][O:25][CH3:26])=[N:17][C:12]=3[CH:13]=[N:14][C:15]=2[CH:16]=1)([CH3:3])[CH3:2].ClC1C=C(C=CC=1)C(OO)=O.C1(C)C=CC(S(Cl)(=O)=O)=CC=1.[OH-].[NH4+:51]>C(Cl)(Cl)Cl>[CH:1]([NH:4][C:5](=[O:27])[O:6][C:7]1[CH:8]=[CH:9][C:10]2[C:11]3[N:19]([CH2:20][CH2:21][CH3:22])[C:18]([CH2:23][CH2:24][O:25][CH3:26])=[N:17][C:12]=3[C:13]([NH2:51])=[N:14][C:15]=2[CH:16]=1)([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 73974-Toluenesulfonyl chlorideHCID 14923Ammonium HydroxideHCID 70297m-Chloroperbenzoic acidHCID 68971459HCID 68971459、化合物

生成物 1

HCID 58833643HCID 58833643、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

2-(2-Methoxyethyl)-1-propyl-1H-imidazo[4,5-c]quinolin-7-yl isopropylcarbamate (1.89 g, 5.10 mmol) was dissolved in chloroform (41 mL). 3-Chloroperoxybenzoic acid (60% pure, 1.60 g, 5.56 mmol) was added in one portion. After 30 minutes the golden solution was diluted with ammonium hydroxide (41 mL), and p-toluenesulfonyl chloride (0.927 g, 4.86 mmol) was added. The reaction was stirred for 1.5 hours. The layers were separated and the aqueous fraction was extracted with dichloromethane. The organic fractions were combined, washed sequentially with water and brine, dried over magnesium sulfate, filtered, and concentrated under reduced pressure. The solid residue was recrystallized from acetonitrile to provide 0.986 g of 4-amino-2-(2-methoxyethyl)-1-propyl-1H-imidazo[4,5-c]quinolin-7-yl isopropylcarbamate as a granular, peach-colored solid, mp 144.0-146.0° C.

後処理

  1. additionwas added
  2. customThe layers were separated
  3. extractionthe aqueous fraction was extracted with dichloromethane
  4. washwashed sequentially with water and brine
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe solid residue was recrystallized from acetonitrile

出典と根拠

ORDレコード
ord-f31747b4681c4543aa09d2a4961eedbb
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08871782B2

反応ノート

読み込み中…

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