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Triethylamine → HCID 19737965、化合物

HRID 2255501
ノート
印刷プレビュー

反応式

HRID 2255501 の反応式
Cl.Cl.[CH3:3][O:4][CH2:5][CH2:6][N:7]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1.C(N(CC)CC)C.[S:20]1[CH:24]=[CH:23][CH:22]=[C:21]1[S:25](Cl)(=[O:27])=[O:26]>C1COCC1>[CH3:3][O:4][CH2:5][CH2:6][N:7]1[CH2:12][CH2:11][N:10]([S:25]([C:21]2[S:20][CH:24]=[CH:23][CH:22]=2)(=[O:27])=[O:26])[CH2:9][CH2:8]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 8471TriethylamineHCID 855182-Thiophenesulfonyl chlorideHCID 21838655HCID 21838655、化合物

生成物 1

HCID 19737965HCID 19737965、化合物収率 75%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of 1-(2-methoxyethyl)piperazine dihydrochloride (2.61 g, 12.0 mmol) in THF (100 mL) was added triethylamine (10 mL) and the resulting mixture was stirred for 10 min. Then a solution of 2-thiophenesulfonyl chloride (1.98 g, 10.84 mmol) was added in THF (3 mL) over 5 min. The reaction mixture was allowed to stir at room temperature for 1 h, the volatiles were evaporated and the residue was extracted with ethyl acetate (3×100 mL). The combined extracts were washed with a saturated sodium bicarbonate solution (50 mL), brine and dried over molecular sieves. Evaporation to dryness gave a viscous oil (2.09 g, 75%).

後処理

  1. stirringto stir at room temperature for 1 h
  2. customthe volatiles were evaporated
  3. extractionthe residue was extracted with ethyl acetate (3×100 mL)
  4. washThe combined extracts were washed with a saturated sodium bicarbonate solution (50 mL), brine
  5. customdried over molecular sieves
  6. customEvaporation to dryness

出典と根拠

ORDレコード
ord-35081c8be57141d6bcda11ba7979ca94
出典データセット
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05240923

反応ノート

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