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4-Toluenesulfonyl chloride → (R)-2-(5-bromo-7-methylquinolin-6-yl)-2-hydroxyethyl 4-methylbenzenesulfonate

HRID 2207044
ノート
印刷プレビュー

反応式

HRID 2207044 の反応式
[Br:1][C:2]1[C:11]([C@@H:12]([OH:15])[CH2:13][OH:14])=[C:10]([CH3:16])[CH:9]=[C:8]2[C:3]=1[CH:4]=[CH:5][CH:6]=[N:7]2.C([Sn](=O)CCCC)CCC.[S:27](Cl)([C:30]1[CH:36]=[CH:35][C:33]([CH3:34])=[CH:32][CH:31]=1)(=[O:29])=[O:28].CCN(CC)CC>C(Cl)Cl>[CH3:34][C:33]1[CH:35]=[CH:36][C:30]([S:27]([O:14][CH2:13][C@@H:12]([C:11]2[C:2]([Br:1])=[C:3]3[C:8](=[CH:9][C:10]=2[CH3:16])[N:7]=[CH:6][CH:5]=[CH:4]3)[OH:15])(=[O:29])=[O:28])=[CH:31][CH:32]=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 8471TriethylamineHCID 61221Dibutyltin oxideHCID 89676590(R)-1-(5-bromo-7-methylquinolin-6-yl)ethane-1,2-diol

生成物 1

HCID 89676717(R)-2-(5-bromo-7-methylquinolin-6-yl)-2-hydroxyethyl 4-methylbenzenesulfonate

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

To a stirred solution of (R)-1-(5-bromo-7-methylquinolin-6-yl)ethane-1,2-diol (197 mg, 0.70 mmol) in CH2Cl2 (97 mL), dibutyltinoxide (3.3 mg, 0.01 mmol), TsCl (150 mg, 0.79 mmol), and Et3N (0.12 mL, 0.83 mmol) were added at 0° C. The reaction mixture was allowed to warm to room temperature overnight. The reaction mixture was quenched with saturated aqueous NH4Cl, and then diluted with CH2Cl2. The organic phase was washed with brine, dried over Na2SO4, filtered and concentrated and purified by flash column chromatography (silica gel, 5 to 100% ethyl acetate/hexanes) to give (R)-2-(5-bromo-7-methylquinolin-6-yl)-2-hydroxyethyl 4-methylbenzenesulfonate. LCMS-ESI+ (m/z): [M+H]+ calc'd for C19H19BrNO4S: 436.02; Found: 436.1.

後処理

  1. customThe reaction mixture was quenched with saturated aqueous NH4Cl
  2. additiondiluted with CH2Cl2
  3. washThe organic phase was washed with brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. custompurified by flash column chromatography (silica gel, 5 to 100% ethyl acetate/hexanes)

出典と根拠

ORDレコード
ord-d4898d60128b41c68d2fa10b54cb95b6
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09376392B2

反応ノート

読み込み中…

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