4-Chlorobutyryl chloride → 7-(4-chlorobutyryl)-2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one

HRID 2294806ノート

反応式

HRID 2294806 の反応式
[S:1]1[C:7]2[S:8][CH:9]=[CH:10][C:6]=2[C:5](=[O:11])[NH:4][CH2:3][CH2:2]1.[Cl:12][CH2:13][CH2:14][CH2:15][C:16](Cl)=[O:17].[Cl-].[Al+3].[Cl-].[Cl-]>ClC(Cl)C>[Cl:12][CH2:13][CH2:14][CH2:15][C:16]([C:9]1[S:8][C:7]2[S:1][CH2:2][CH2:3][NH:4][C:5](=[O:11])[C:6]=2[CH:10]=1)=[O:17]

参加物

5

反応物 3

HCID 783704-Chlorobutyryl chlorideHCID 43659423,4-dihydrothieno[3,2-f][1,4]thiazepin-5(2H)-oneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 214720567-(4-chlorobutyryl)-2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one収率 59%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

To a mixture of 13 g of 2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one and 21.5 g of 4-chlorobutyryl chloride in 200 ml of dichloroethane was added 21.5 g of aluminum chloride under cooling and the mixture was stirred for 3 hours. The mixture was poured into ice-cold water and extracted with chloroform. The organic layer was washed with saline solution, dried over magnesium sulfate and concentrated. The residue was recrystallized from ethanol to give 12 g of 7-(4-chlorobutyryl)-2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one as white crystals, m.p. 124°-125° C.

後処理

  1. temperatureunder cooling
  2. additionThe mixture was poured into ice-cold water
  3. extractionextracted with chloroform
  4. washThe organic layer was washed with saline solution
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated
  7. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-4fe21fffeb3b499886d0dd311c14643d
出典データセット
uspto-grants-1997_11
特許番号
US05691330

反応ノート

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