Water → 4-(4-Cyanophenyl)-4-[4-(tetrahydro-2h-pyran-2-yloxy)phenoxy]butyl methanesulfonate

HRID 411539노트

반응식

HRID 411539 반응식
[OH:1][CH2:2][CH2:3][CH2:4][CH:5]([C:20]1[CH:27]=[CH:26][C:23]([C:24]#[N:25])=[CH:22][CH:21]=1)[O:6][C:7]1[CH:12]=[CH:11][C:10]([O:13][CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][O:15]2)=[CH:9][CH:8]=1.[CH3:28][S:29](Cl)(=[O:31])=[O:30].O>C(Cl)Cl>[CH3:28][S:29]([O:1][CH2:2][CH2:3][CH2:4][CH:5]([C:20]1[CH:27]=[CH:26][C:23]([C:24]#[N:25])=[CH:22][CH:21]=1)[O:6][C:7]1[CH:8]=[CH:9][C:10]([O:13][CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][O:15]2)=[CH:11][CH:12]=1)(=[O:31])=[O:30]

참가 물질

5

반응물 3

HCID 962WaterHCID 31297Methanesulfonyl chlorideHCID 222354084-{4-Hydroxy-1-[4-(tetrahydro-2h-pyran-2-yloxy)phenoxy]butyl}-benzonitrile

생성물 1

HCID 222355174-(4-Cyanophenyl)-4-[4-(tetrahydro-2h-pyran-2-yloxy)phenoxy]butyl methanesulfonate수율 100%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

A solution of 4-{4-hydroxy-1-[4-(tetrahydro-2H-pyran-2-yloxy)phenoxy]butyl}benzonitrile (see step (ii) above; 2.37 g, 6.45 mmol) and TEA (1.35 mL, 9.68 mmol) in DCM (10 mL) was cooled to −5° C. Methanesulfonyl chloride (0.65 mL, 8.38 mmol) in DCM (5 mL) was added slowly. After addition was complete, the temperature was maintained below 5° C. for 1 h before DCM and water were added. The organic layer was washed with water, dried (Na2SO4) and then evaporated to yield 2.87 g (100%) of the sub-title compound. This was used in the next step without further purification.

후처리

  1. additionAfter addition
  2. additionwere added
  3. washThe organic layer was washed with water
  4. dry with materialdried (Na2SO4)
  5. customevaporated

출처 및 근거

ORD 기록
ord-9b277457e9dd45738393983307b63d40
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06559162B2

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