Acetone → Brl 16657

HRID 26282

反応式

HRID 26282 の反応式
Cl.[CH3:2][N:3]([CH2:5][CH2:6][Cl:7])[CH3:4].[F:8][C:9]([F:28])([F:27])[C:10]1[CH:15]=[CH:14][C:13]([CH:16]2[CH2:25][CH2:24][C:23]3[C:18](=[CH:19][C:20](O)=CC=3)[O:17]2)=[CH:12][CH:11]=1.[C:29](=O)([O-])[O-].[K+].[K+].[I-].[K+].[CH3:37][C:38]([CH3:40])=[O:39]>CCOCC>[ClH:7].[CH3:37][C:38]1([CH3:29])[CH2:40][CH:16]([C:13]2[CH:12]=[CH:11][C:10]([C:9]([F:8])([F:27])[F:28])=[CH:15][CH:14]=2)[C:25]2[C:24](=[CH:23][C:18]([O:17][CH2:6][CH2:5][N:3]([CH3:4])[CH3:2])=[CH:19][CH:20]=2)[O:39]1

参加物

7

反応物 5

HCID 180AcetoneHCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 11636816N,N-Dimethylaminoethyl chloride hydrochlorideHCID 867355634-Trifluoromethylphenylchroman-7-ol

生成物 1

HCID 42989Brl 16657

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

Dimethylaminoethylchloride hydrochloride (1.5 g) was added to 2,2-dimethyl-4-(4-trifluoromethylphenylchroman-7-ol (1.0 g), potassium carbonate (4.0 g) and potassium iodide (1.5 g) in acetone (50 ml) and the mixture refluxed for 2 days. The mixture was filtered and the acetone was evaporated under reduced pressure. The resulting crude oil was chromatographed on alumina. Elution with ether:petrol (1:1) gave a clear oil which after dissolution in dry ether and passage of dry halogen chloride through the solution yielded the required chroman as the hydrochloride salt (0.35 g), m.p. 200°-203° C.

後処理

  1. temperaturethe mixture refluxed for 2 days
  2. filtrationThe mixture was filtered
  3. customthe acetone was evaporated under reduced pressure
  4. customThe resulting crude oil was chromatographed on alumina
  5. washElution with ether:petrol (1:1)
  6. customgave a clear oil which

出典と根拠

ORDレコード
ord-3373465bb8a242568b7f601f92f97f86
出典データセット
uspto-grants-1979_04
特許番号
US04148909

関連ノート

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