Iodine → HCID 14628034, 화합물

HRID 1199106노트

반응식

HRID 1199106 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 14628034HCID 14628034, 화합물수율 36.8%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a32e06e5b0a64903932cdc0e84df2386
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04898943

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