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Methylamine → 1-Amino-2-(2-fluorobenzoyl)pyrrole

HRID 280115
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반응식

HRID 280115 반응식
[F:1][C:2]1[CH:25]=[CH:24][CH:23]=[CH:22][C:3]=1[C:4]([C:6]1[N:7]([N:11]2C(=O)C3=CC=CC=C3C2=O)[CH:8]=[CH:9][CH:10]=1)=[O:5].CN>CN(C=O)C.O>[NH2:11][N:7]1[CH:8]=[CH:9][CH:10]=[C:6]1[C:4](=[O:5])[C:3]1[CH:22]=[CH:23][CH:24]=[CH:25][C:2]=1[F:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 6329MethylamineHCID 134577152-(2-Fluorobenzoyl)-1-phthalimidopyrrole

생성물 1

HCID 134577161-Amino-2-(2-fluorobenzoyl)pyrrole수율 93%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a suspension of 2-(2-fluorobenzoyl)-1-phthalimidopyrrole (12.5 g, 27 mmole) in 40 ml DMF was added 40 ml methylamine (40% solution in water). After stirring one hour at ambient temperature, the reaction mixture was diluted with water and extracted with ether. The organic extract was washed with water and with saturated NaCl solution, dried over anhydrous MgSO4, filtered and evaporated to 9 L g oil, half of which was purified by Kugelrohr distillation (120°-130° at 0.2 mm Hg) to give 3.5 g (93%) solid, m.p. 44°-47°.

후처리

  1. extractionextracted with ether
  2. extractionThe organic extract
  3. washwas washed with water and with saturated NaCl solution
  4. dry with materialdried over anhydrous MgSO4
  5. filtrationfiltered
  6. customevaporated to 9 L g oil, half of which
  7. distillationwas purified by Kugelrohr distillation (120°-130° at 0.2 mm Hg)

출처 및 근거

ORD 기록
ord-dc1a0d691de7435da2494afb2f5a93d6
출처 데이터셋
uspto-grants-1986_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04588727

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