Formamidine acetate → HCID 178419030、化合物

HRID 6823

反応式

HRID 6823 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 178419030HCID 178419030、化合物収率 91.2%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
110 °C

実験手順

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).

後処理

  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.

出典と根拠

ORDレコード
ord-0d4cdbe90b8748d0ab8949e429a5dc83
出典データセット
uspto-grants-2006_08
特許番号
US07084147B2

関連ノート

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