Ethanethiol → HCID 10397992、化合物

HRID 976349ノート

反応式

HRID 976349 の反応式
C(S)C.[Cl-].[Al+3].[Cl-].[Cl-].[CH:8]([C:11]1[CH:12]=[C:13]2[C:18](=[CH:19][C:20]=1[O:21]C)[C:17](=[O:23])[CH2:16][CH2:15][CH2:14]2)([CH3:10])[CH3:9]>ClCCl>[OH:21][C:20]1[CH:19]=[C:18]2[C:13]([CH2:14][CH2:15][CH2:16][C:17]2=[O:23])=[CH:12][C:11]=1[CH:8]([CH3:10])[CH3:9]

参加物

5

反応物 3

HCID 6343EthanethiolHCID 6451240Aluminum(III) ChlorideHCID 101048026-Isopropyl-7-methoxy-1-tetralone

生成物 1

HCID 10397992HCID 10397992、化合物収率 59.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

20 ml of ethanethiol was added to 100 ml of a suspension of 28 g of aluminium chloride in dichloromethane cooled with ice. The obtained mixture was stirred for 5 minutes, followed by the slowly, dropwise addition thereto of 50 ml of a solution of 15.3 g of 6-isopropyl-7-methoxy-1-tetralone in dichloromethane. After the completion of the dropwise addition, the obtained mixture was stirred for 3 hours at room temperature and poured onto ice-water. The obtained mixture was extracted with ethyl acetate. The organic phase was washed with water, a saturated aqueous solution of sodium hydrogencarbonate and a saturated aqueous solution of common salt successively, dried over anhydrous magnesium sulfate, and distilled to remove the solvent. The obtained solid residue was washed with n-hexane to give 8.5 g of the title compound as a white solid.

後処理

  1. temperaturecooled with ice
  2. additiondropwise addition
  3. additionAfter the completion of the dropwise addition
  4. stirringthe obtained mixture was stirred for 3 hours at room temperature
  5. additionpoured onto ice-water
  6. extractionThe obtained mixture was extracted with ethyl acetate
  7. washThe organic phase was washed with water
  8. dry with materiala saturated aqueous solution of sodium hydrogencarbonate and a saturated aqueous solution of common salt successively, dried over anhydrous magnesium sulfate
  9. distillationdistilled
  10. customto remove the solvent
  11. washThe obtained solid residue was washed with n-hexane

出典と根拠

ORDレコード
ord-c1470c553ca347e2acb54823493d176f
出典データセット
uspto-grants-1997_03
特許番号
US05612356

反応ノート

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