Pyridine → HCID 53726966、化合物

HRID 614009ノート

反応式

HRID 614009 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[O:9][CH:8]([CH3:10])[CH2:7][C:6]2=[C:11]([NH2:13])[CH:12]=1.N1C=CC=CC=1.[CH2:20]([S:29](Cl)(=[O:31])=[O:30])[C:21]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)=[O:22]>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:12]=[C:11]([NH:13][S:29]([CH2:20][C:21]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[O:22])(=[O:31])=[O:30])[C:6]2[CH2:7][CH:8]([CH3:10])[O:9][C:5]=2[CH:4]=1

参加物

5

反応物 3

HCID 1049PyridineHCID 122818442-Oxo-2-phenyl-ethanesulfonyl chlorideHCID 213298112,3-Dihydro-6-methoxy-2-methyl-4-benzofuranamine

生成物 1

HCID 53726966HCID 53726966、化合物収率 51.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 15.5 grams of 2,3-dihydro-6-methoxy-2-methyl-4-benzofuranamine and 10.5 grams of anhydrous pyridine in 100 cc of methylene chloride cooled to 0°-5° C., a solution of 24.5 grams of phenacylsulfonyl chloride in 80 cc of methylene chloride is added. When the dripping is terminated the reaction mixture is warmed to room temperature and stirred for 5 hours. At the end of this time the solution is washed with water, dried over sodium sulfate and concentrated to dryness. Crystallization of the resulting thick oil from ethyl alcohol-ethyl ether gives 16 grams of the compound of the title which melts at 143°-145° C.

後処理

  1. customWhen the dripping is terminated the reaction mixture
  2. washAt the end of this time the solution is washed with water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated to dryness
  5. customCrystallization of the resulting thick oil from ethyl alcohol-ethyl ether

出典と根拠

ORDレコード
ord-5b737da5db70441ab59ff7293b24faf0
出典データセット
uspto-grants-1979_03
特許番号
US04143055

反応ノート

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