4-Toluenesulfonyl chloride → HCID 57583239, 화합물

HRID 1645498노트

반응식

HRID 1645498 반응식
[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]

참가 물질

4

반응물 2

HCID 73974-Toluenesulfonyl chlorideHCID 10898853HCID 10898853, 화합물

생성물 1

HCID 57583239HCID 57583239, 화합물수율 60%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-02eff92c761044f4921caafc2166c6c2
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08124806B2

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