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Pyridine → 6-Decyl-3-methylthio-2-(trifluoromethanesulfonyloxy)naphthalene

HRID 1476373
ノート
印刷プレビュー

反応式

HRID 1476373 の反応式
FC(F)(F)S([O:6][S:7]([C:10]([F:13])([F:12])[F:11])(=[O:9])=[O:8])(=O)=O.ClCCl.[CH2:19]([C:29]1[CH:30]=[C:31]2[C:36](=[CH:37][CH:38]=1)[CH:35]=[C:34](O)[C:33]([S:40][CH3:41])=[CH:32]2)[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28].N1C=CC=CC=1>O.Cl>[CH2:19]([C:29]1[CH:30]=[C:31]2[C:36](=[CH:37][CH:38]=1)[CH:35]=[C:34]([O:6][S:7]([C:10]([F:11])([F:12])[F:13])(=[O:8])=[O:9])[C:33]([S:40][CH3:41])=[CH:32]2)[CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 1049PyridineHCID 6344DichloromethaneHCID 67749Trifluoromethanesulfonic anhydrideHCID 867043886-Decyl-3-methylthio-2-hydroxynaphthalene

生成物 1

HCID 867043896-Decyl-3-methylthio-2-(trifluoromethanesulfonyloxy)naphthalene収率 105.7%

試薬・触媒・溶媒 2

HCID 313
Hydrochloric Acid
溶媒
HCID 962Water溶媒

実験手順

Trifluoromethanesulfonic anhydride (3 ml, 15 mmol) was added to a dichloromethane (50 ml) solution of the obtained 6-decyl-3-methylthio-2-hydroxynaphthalene (3.63 g, 10 mmol) and pyridine (2.5 ml, 30 mmol) at 0° C. This solution was stirred at room temperature for 25 minutes. Then, the mixture was diluted with water (20 ml), and hydrochloric acid (4 M, 20 ml) was added. The mixture was extracted with dichloromethane (30 ml×3). The organic phases obtained by repeating the extraction three times were collected, washed with saturated saline water (30 ml×3), dried with MgSO4, and condensed to obtain 6-decyl-3-methylthio-2-(trifluoromethanesulfonyloxy)naphthalene (compound (4)-81) (4.89 g, 99%).

後処理

  1. additionwas added
  2. extractionThe mixture was extracted with dichloromethane (30 ml×3)
  3. customThe organic phases obtained
  4. extractionthe extraction three times
  5. customwere collected
  6. washwashed with saturated saline water (30 ml×3)
  7. dry with materialdried with MgSO4, and condensed

出典と根拠

ORDレコード
ord-ed4e1ddcc0824711a242da0d5b994ca5
出典データセット
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09018630B2

反応ノート

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