Sodium Hydroxide → HCID 13534713, 화합물

HRID 4362

반응식

HRID 4362 반응식
Cl.[NH2:2][N:3]1[CH2:8][CH:7]=[C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:5][CH2:4]1.[OH-].[Na+].[F:17][C:18]1[CH:23]=[CH:22][C:21]([N:24]=[C:25]=[S:26])=[CH:20][CH:19]=1>O1CCOCC1.O>[F:17][C:18]1[CH:23]=[CH:22][C:21]([NH:24][C:25]([NH:2][N:3]2[CH2:4][CH:5]=[C:6]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)[CH2:7][CH2:8]2)=[S:26])=[CH:20][CH:19]=1

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 152414-Fluorophenyl isothiocyanateHCID 20152381N-amino-4-phenyl-1,2,3,6-tetrahydropyridine hydrochloride

생성물 1

HCID 13534713HCID 13534713, 화합물수율 64.4%

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매2회

실험 절차

To a stirred solution of N-amino-4-phenyl-1,2,3,6-tetrahydropyridine hydrochloride (1.05 g) in a mixture of dioxane (10 ml) and water (5 ml) was added 1N sodium hydroxide solution (5 ml) under ice-bath cooling, and then a solution of 4-fluorophenyl isothiocyanate (1.15 g) in dioxane (5 ml) was added thereto. The mixture was stirred for 5 hours under ice-bath cooling. The reaction mixture was evaporated in vacuo and the residue was extracted several times with ethyl acetate. The combined extract was washed with water, dried over magnesium sulfate and evaporated in vacuo to give a crude product, which was recrystallized from ethyl acetate to give N-[[(4-fluorophenyl)thiocarbamoyl]amino]-4-phenyl-1,2,3,6-tetrahydropyridine (1.05 g).

후처리

  1. temperaturecooling
  2. temperaturecooling
  3. customThe reaction mixture was evaporated in vacuo
  4. extractionthe residue was extracted several times with ethyl acetate
  5. extractionThe combined extract
  6. washwas washed with water
  7. dry with materialdried over magnesium sulfate
  8. customevaporated in vacuo
  9. customto give a crude product, which
  10. customwas recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-2972a999c99c4df9bc9aa7a812034758
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04725608

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