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4-Toluenesulfonyl chloride → HCID 58380558、化合物

HRID 1259412
ノート
印刷プレビュー

反応式

HRID 1259412 の反応式
[O:1]1[CH2:4][CH:3]([CH2:5][CH2:6][OH:7])[CH2:2]1.[C:8]1([CH3:18])[CH:13]=[CH:12][C:11]([S:14](Cl)(=[O:16])=[O:15])=[CH:10][CH:9]=1>N1C=CC=CC=1>[CH3:18][C:8]1[CH:13]=[CH:12][C:11]([S:14]([O:7][CH2:6][CH2:5][CH:3]2[CH2:4][O:1][CH2:2]2)(=[O:16])=[O:15])=[CH:10][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 73974-Toluenesulfonyl chlorideHCID 108443452-(Oxetan-3-yl)ethan-1-ol

生成物 1

HCID 58380558HCID 58380558、化合物収率 56.2%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Using the same reaction conditions and procedure as described for the preparation of Intermediate (I-16a), 2-(oxetan-3-yl)ethanol (1 g, 6.944 mmol) was reacted with p-Toluene sulfonyl chloride (1.9 g, 10.416 mmol) in dry pyridine (10 mL) to afford the crude product. The reaction mass was poured into ice-water and extracted using ethyl acetate. The organic layer was washed with 1N HCl, brine solution, dried over anhydrous sodium sulfate and concentrated under reduced pressure to afford the crude product. Purification by column chromatography on silica gel (20% ethyl acetate in hexane) afforded 1 g of the product (40% yield).

後処理

  1. customthe same reaction conditions and procedure
  2. customto afford the crude product
  3. extractionextracted
  4. washThe organic layer was washed with 1N HCl, brine solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customto afford the crude product
  8. customPurification by column chromatography on silica gel (20% ethyl acetate in hexane)

出典と根拠

ORDレコード
ord-25a6addfa0b04fc1b7f5f7ab3a18309c
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08466289B2

反応ノート

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