Iodine → HCID 14628034、化合物

HRID 1199106ノート

反応式

HRID 1199106 の反応式
[CH:1]1([CH2:7][CH2:8][CH2:9][C:10](=O)[CH3:11])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[NH2:13][C:14]([NH2:16])=[S:15].II.[OH-].[Na+]>O>[CH:1]1([CH2:7][CH2:8][C:9]2[S:15][C:14]([NH2:16])=[N:13][C:10]=2[CH3:11])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

6

反応物 4

HCID 807IodineHCID 14798Sodium HydroxideHCID 2723790ThioureaHCID 135556845-Cyclohexylpentan-2-one

生成物 1

HCID 14628034HCID 14628034、化合物収率 36.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 22.2 g of 5-cyclohexyl-2-pentanone, 20.10 g of thiourea, and 33.48 g of iodine was stirred for 23 hours at a bath temperature of from 100° to 120° C. To the mixture was added 150 ml of water, followed by refluxing for 30 minutes. After cooling, an aqueous sodium hydroxide solution was added to neutralize. The mixture was extracted with ethyl acetate, and the extract was washed with water and dried. The solvent was removed by distillation, and the residue was purified by silica gel column chromatography. Recrystallization from aqueous methanol yielded 10.9 g of the titled compound.

後処理

  1. temperatureby refluxing for 30 minutes
  2. temperatureAfter cooling
  3. extractionThe mixture was extracted with ethyl acetate
  4. washthe extract was washed with water
  5. customdried
  6. customThe solvent was removed by distillation
  7. customthe residue was purified by silica gel column chromatography
  8. customRecrystallization from aqueous methanol

出典と根拠

ORDレコード
ord-a32e06e5b0a64903932cdc0e84df2386
出典データセット
uspto-grants-1990_02
特許番号
US04898943

反応ノート

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