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Sulfuric Acid → HCID 18691297、化合物

HRID 1871458
ノート
印刷プレビュー

反応式

HRID 1871458 の反応式
COC1C=CC(C[NH:8][C:9]2[C:14]3[CH:15]=[CH:16][S:17][C:13]=3[CH:12]=[C:11]([CH3:18])[N:10]=2)=CC=1.S(=O)(=O)(O)O.O.N>FC(F)(F)C(O)=O>[NH2:8][C:9]1[C:14]2[CH:15]=[CH:16][S:17][C:13]=2[CH:12]=[C:11]([CH3:18])[N:10]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 12896473Azane;hydrateHCID 18691200HCID 18691200、化合物

生成物 1

HCID 18691297HCID 18691297、化合物収率 108.2%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

To a solution of 24 g of 4-(4-methoxybenzyl)amino-6-methylthieno[3,2-c]pyridine in 80 ml of trifluoroacetic acid was added 15 ml of concentrated sulfuric acid, and the mixture was stirred at ambient temperature for 30 minutes. The reaction mixture was poured into ice water, rendered alkaline by the addition of 28% ammonia water and extracted with chloroform. The extract was washed with water and saturated saline, dried over anhydrous magnesium sulfate. The drying agent was removed by filtration, and the solvent was removed under reduced pressure. The residue was purified by column chromatography on silica gel and recrystallized from chloroform/petroleum ether to give 15 g of the title compound as a white powder.

後処理

  1. extractionextracted with chloroform
  2. washThe extract was washed with water and saturated saline
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe drying agent was removed by filtration
  5. customthe solvent was removed under reduced pressure
  6. customThe residue was purified by column chromatography on silica gel
  7. customrecrystallized from chloroform/petroleum ether

出典と根拠

ORDレコード
ord-cf8a147536b241b491dca875f5e82397
出典データセット
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06103736

反応ノート

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