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4-Toluenesulfonyl chloride → HCID 67052431、化合物

HRID 599435
ノート
印刷プレビュー

反応式

HRID 599435 の反応式
C1C=C(Cl)C=C(C(OO)=O)C=1.O=C1C2C(=CC=CC=2)C(=O)[N:14]1[O:23][CH2:24][C:25]1[N:26]([CH2:38][CH2:39][CH2:40][NH:41][C:42](=[O:48])[O:43][C:44]([CH3:47])([CH3:46])[CH3:45])[C:27]2[C:36]3[N:35]=[CH:34][CH:33]=[CH:32][C:31]=3[N:30]=[CH:29][C:28]=2[N:37]=1.[OH-].[NH4+:50].C1(C)C=CC(S(Cl)(=O)=O)=CC=1>C(Cl)(Cl)Cl>[NH2:50][C:29]1[C:28]2[N:37]=[C:25]([CH2:24][O:23][NH2:14])[N:26]([CH2:38][CH2:39][CH2:40][NH:41][C:42](=[O:48])[O:43][C:44]([CH3:45])([CH3:47])[CH3:46])[C:27]=2[C:36]2[N:35]=[CH:34][CH:33]=[CH:32][C:31]=2[N:30]=1
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 67052435HCID 67052435、化合物

生成物 1

HCID 67052431HCID 67052431、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

mCPBA (2.33 g, 13.5 mmol) was added to a suspension of tert-butyl 3-(2-{[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)oxy]methyl}-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl)propylcarbamate (4.86 g, 9.67 mmol) in chloroform (50 mL). The reaction mixture was allowed to stir for 4 hours, then concentrated ammonium hydroxide (27 mL) and p-toluenesulfonyl chloride (2.03 g, 10.6 mmol) were added. The reaction mixture was allowed to stir overnight at room temperature, then was filtered. The filtrate was diluted with saturated aqueous sodium bicarbonate (50 mL) and extracted with chloroform (2×40 mL). The organic layers were combined, dried over magnesium sulfate, filtered, and concentrated to afford a brown solid that was purified by chromatography using a HORIZON HPFC system (silica gel, gradient elution with 0-30% CMA in chloroform) to afford 1.00 g of tert-butyl 3-{4-amino-2-[(aminooxy)methyl]-1H-imidazo[4,5-c][1,5]naphthyridin-1-yl}propylcarbamate as a yellow solid that contained some minor impurities.

後処理

  1. stirringto stir overnight at room temperature
  2. filtrationwas filtered
  3. additionThe filtrate was diluted with saturated aqueous sodium bicarbonate (50 mL)
  4. extractionextracted with chloroform (2×40 mL)
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customto afford a brown solid that
  9. customwas purified by chromatography
  10. washa HORIZON HPFC system (silica gel, gradient elution with 0-30% CMA in chloroform)

出典と根拠

ORDレコード
ord-126ebde67349422693cffff05729ce38
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07897767B2

反応ノート

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