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Potassium Carbonate → 3,4-Dimethyl-7-(2-methyl-1,3,4-thiadiazol-5-yl)-methoxycoumarin

HRID 1460985
ノート
印刷プレビュー

反応式

HRID 1460985 の反応式
O[C:2]1[CH:11]=[C:10]2[C:5]([C:6]([CH3:14])=[C:7]([CH3:13])[C:8](=[O:12])[O:9]2)=[CH:4][CH:3]=1.Cl[CH2:16][C:17]1[S:18][C:19](C)=[N:20][N:21]=1.[C:23]([O-])([O-])=[O:24].[K+].[K+]>CC(C)=O>[CH3:13][C:7]1[C:8](=[O:12])[O:9][C:10]2[C:5]([C:6]=1[CH3:14])=[C:4]([O:24][CH3:23])[CH:3]=[C:2]([C:19]1[S:18][C:17]([CH3:16])=[N:21][N:20]=1)[CH:11]=2
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 54129907-hydroxy-3,4-dimethyl-2H-chromen-2-oneHCID 155820072-(Chloromethyl)-5-methyl-1,3,4-thiadiazole

生成物 1

HCID 197514973,4-Dimethyl-7-(2-methyl-1,3,4-thiadiazol-5-yl)-methoxycoumarin

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 5.0 g of 7-hydroxy-3,4-dimethylcoumarin, 3.9 g of 2-chloromethyl-5-methyl-1,3,4-thiadiazole, 3.5 g of K2CO3 and 100 ml of acetone was refluxed for 20 hours and evaporated down, and the residue was partitioned in H2O/methylene chloride. After the undissolved constituents had been separated off, the organic phase was washed once with 1N NaOH and then with H2O, dried over Na2SO4 and evaporated down, and the residue was recrystallized from methanol and dried.

後処理

  1. temperaturewas refluxed for 20 hours
  2. customevaporated down
  3. customthe residue was partitioned in H2O/methylene chloride
  4. customAfter the undissolved constituents had been separated off
  5. washthe organic phase was washed once with 1N NaOH
  6. dry with materialwith H2O, dried over Na2SO4
  7. customevaporated down
  8. customthe residue was recrystallized from methanol
  9. customdried

出典と根拠

ORDレコード
ord-2648e61e93704d1a87ed81403a8e0bdd
出典データセット
uspto-grants-1991_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05073563

反応ノート

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