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Potassium Carbonate → N-[4-chloro-3-(3-methoxy-5,6-dihydro-2H-thiopyranyl)-phenyl]-3,4,5,6-tetrahydrophthalimide

HRID 727748
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HRID 727748 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11]3[CH2:14][CH2:15][CH2:16][CH2:17][C:10]=3[C:9]2=[O:18])=[CH:4][C:3]=1O.ClC[C:22]1[CH2:23][S:24][CH2:25][CH2:26][CH:27]=1.[C:28](=O)([O-])[O-:29].[K+].[K+]>C(#N)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11]3[CH2:14][CH2:15][CH2:16][CH2:17][C:10]=3[C:9]2=[O:18])=[CH:4][C:3]=1[CH:23]1[C:22]([O:29][CH3:28])=[CH:27][CH2:26][CH2:25][S:24]1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 12769235N-(3-Hydroxy-4-chlorophenyl)-3,4,5,6-tetrahydrophthalimideHCID 156145643-chloromethyl-5,6-dihydro-2H-thiopyran

생성물 1

HCID 22617247N-[4-chloro-3-(3-methoxy-5,6-dihydro-2H-thiopyranyl)-phenyl]-3,4,5,6-tetrahydrophthalimide

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

13.9 g of N-(4-chloro-3-hydroxyphenyl)-3,4,5,6-tetrahydrophthalimide, 8.2 9 of 3-chloromethyl-5,6-dihydro-2H-thiopyran and 8.3 g of potassium carbonate in 150 ml of acetonitrile are refluxed for hours. The mixture is cooled and filtered, the filtrate is evaporated down, the residue is taken up in 200 ml of methylene chloride and the solution is washed twice with 10% strength sodium hydroxide solution and 3 times with water, dried and evaporated out. 15.0 g of N-[4-chloro-3-(3-methoxy-5,6-dihydro-2H-thiopyranyl)-phenyl]-3,4,5,6-tetrahydrophthalimide (mp. 116-119° C.) are obtained. ##STR20##

후처리

  1. temperatureThe mixture is cooled
  2. filtrationfiltered
  3. customthe filtrate is evaporated down
  4. washthe solution is washed twice with 10% strength sodium hydroxide solution and 3 times with water
  5. customdried
  6. customevaporated out

출처 및 근거

ORD 기록
ord-88383c4fbf9b479f95587f7cff4b6d1d
출처 데이터셋
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05045105

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