Ammonium Chloride → HCID 86650697, 화합물

HRID 1873686노트

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HRID 1873686 반응식
[F:1][C:2]1[CH:27]=[C:26]([N+:28]([O-])=O)[CH:25]=[CH:24][C:3]=1[O:4][C:5]1[C:14]2[C:9](=[CH:10][C:11]([O:22][CH3:23])=[C:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH:13]=2)[N:8]=[CH:7][CH:6]=1.[Cl-].[NH4+]>O.C(O)C.[Fe]>[NH2:28][C:26]1[CH:25]=[CH:24][C:3]([O:4][C:5]2[C:14]3[C:9](=[CH:10][C:11]([O:22][CH3:23])=[C:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH:13]=3)[N:8]=[CH:7][CH:6]=2)=[C:2]([F:1])[CH:27]=1

참가 물질

5

반응물 2

HCID 25517Ammonium ChlorideHCID 86650695HCID 86650695, 화합물

생성물 1

HCID 86650697HCID 86650697, 화합물수율 93%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 19096565Water ethanol용매

반응 조건

온도
80 °C

실험 절차

Compound 1b (400 mg) was dissolved in a water-ethanol (1:1) mixture (10 mL), and iron powder (1.0 g) and ammonium chloride (1.0 g) were added thereto, followed by stirring at 80° C. for 2 hours. The reaction mixture was filtered through Celite to thereby remove iron powder, and water (100 mL) was added to the filtrate, followed by extraction with ethyl acetate (50 mL). The organic phase was washed with saturated brine (100 mL) and dried over sodium sulfate, followed by concentration under reduced pressure, to thereby yield compound 1c (335 mg, yield: 93%).

후처리

  1. additionwere added
  2. filtrationThe reaction mixture was filtered through Celite to thereby remove iron powder, and water (100 mL)
  3. additionwas added to the filtrate
  4. extractionfollowed by extraction with ethyl acetate (50 mL)
  5. washThe organic phase was washed with saturated brine (100 mL)
  6. dry with materialdried over sodium sulfate
  7. concentrationfollowed by concentration under reduced pressure

출처 및 근거

ORD 기록
ord-0d21da34e8b747d3a19befdc562a65fa
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08304427B2

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