4-Toluenesulfonyl chloride → HCID 57583239、化合物

HRID 1645498ノート

反応式

HRID 1645498 の反応式
[OH:1][CH2:2][CH:3]([CH2:7][CH2:8][CH2:9][OH:10])[CH2:4][CH2:5][OH:6].[C:11]1([CH3:21])[CH:16]=[CH:15][C:14]([S:17](Cl)(=[O:19])=[O:18])=[CH:13][CH:12]=1>N1C=CC=CC=1>[S:17]([O:6][CH2:5][CH2:4][CH:3]([CH2:2][O:1][S:17]([C:14]1[CH:15]=[CH:16][C:11]([CH3:21])=[CH:12][CH:13]=1)(=[O:19])=[O:18])[CH2:7][CH2:8][CH2:9][O:10][S:17]([C:14]1[CH:15]=[CH:16][C:11]([CH3:21])=[CH:12][CH:13]=1)(=[O:19])=[O:18])([C:14]1[CH:15]=[CH:16][C:11]([CH3:21])=[CH:12][CH:13]=1)(=[O:19])=[O:18]

参加物

4

反応物 2

HCID 73974-Toluenesulfonyl chlorideHCID 10898853HCID 10898853、化合物

生成物 1

HCID 57583239HCID 57583239、化合物収率 60%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 3-hydroxymethylhexane-1,6-diol (4 g, 0.027 mol) in pyridine (80 mL) stirred in an ice bath was added para-toluenesulphonyl chloride (16.9 g, 0.09 mol) in one portion. The mixture was allowed to warm to ambient temperature. After 48 hours the reaction was worked up using DCM (100 mL) which was washed with 1N HCl (2×100 mL). The organic layer was dried and concentrated to yield a very viscous, sticky oil which was analysed by NMR. This confirmed the desired material had been formed in a yield of 60% (9.9 g). The material was used without further purification.

後処理

  1. washDCM (100 mL) which was washed with 1N HCl (2×100 mL)
  2. customThe organic layer was dried
  3. concentrationconcentrated
  4. customto yield a very viscous, sticky oil which
  5. customhad been formed in a yield of 60% (9.9 g)
  6. customThe material was used without further purification

出典と根拠

ORDレコード
ord-02eff92c761044f4921caafc2166c6c2
出典データセット
uspto-grants-2012_02
特許番号
US08124806B2

反応ノート

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