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

HRID 462739
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반응식

HRID 462739 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 g oil, half of which was purified by Kugelrohr distallation (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 g oil, half of which
  7. customwas purified by Kugelrohr distallation (120°-130° at 0.2 mm Hg)

출처 및 근거

ORD 기록
ord-064dc037ee864b59b224eb94988adb36
출처 데이터셋
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04517195

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