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

HRID 841843
ノート
印刷プレビュー

反応式

HRID 841843 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ae77e55afd61442eb35d21089d65bfb5
出典データセット
uspto-grants-2002_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
USRE037664E1

反応ノート

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