Formamidine acetate → HCID 178419030, 화합물

HRID 6823

반응식

HRID 6823 반응식
[F:1][C:2]1[CH:3]=[C:4]2[NH:10][C:9](=O)O[C:6](=[O:7])[C:5]2=[CH:12][C:13]=1[I:14].C(O)(=O)C.C(N)=[NH:20]>CN(C)C=O>[OH:7][C:6]1[C:5]2[C:4](=[CH:3][C:2]([F:1])=[C:13]([I:14])[CH:12]=2)[N:10]=[CH:9][N:20]=1

참가 물질

4

반응물 2

HCID 160693Formamidine acetateHCID 543357764-Fluoro-5-iodo-isatoic Anhydride

생성물 1

HCID 178419030HCID 178419030, 화합물수율 91.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
110 °C

실험 절차

Dimethylformamide (0.5 litres), 4-fluoro-5-iodo-isatoic anhydride (45 grams, 147 mmoles), and formamidine acetate (45.92 grams, 441 mmoles), were combined in a one litre one-neck flask fitted with a magnetic stir bar. The mixture was placed under anhydrous nitrogen and heated at 110° C. for 6 hours. The mixture was allowed to cool, followed by concentrating the reaction mixture to one third its original volume on the rotary evaporator. The resulting mixture was poured onto 3 litres of ice water. The resulting precipitated solid was collected by suction filtration. The solid was washed with an additional one litre of distilled water. The resulting solid was dried under vacuum at 70° C. to yield 38.9 grams (91%) of the title compound. 1H NMR (400 MHz, DMSO-d6) δ: 12.43(s, 1H), 8.46(d, 1H), 8.12(s, 1H), 7.49(d, 1H). ESI-MS m/z 291 (M+1).

후처리

  1. customfitted with a magnetic stir bar
  2. temperatureto cool
  3. concentrationby concentrating the reaction mixture to one third its original volume
  4. customon the rotary evaporator
  5. additionThe resulting mixture was poured onto 3 litres of ice water
  6. customThe resulting precipitated solid
  7. filtrationwas collected by suction filtration
  8. washThe solid was washed with an additional one litre of distilled water
  9. customThe resulting solid was dried under vacuum at 70° C.

출처 및 근거

ORD 기록
ord-0d4cdbe90b8748d0ab8949e429a5dc83
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07084147B2

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