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Pyridine → HCID 19737610、化合物

HRID 2255650
ノート
印刷プレビュー

反応式

HRID 2255650 の反応式
[I:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[CH:4][CH:3]=1.[I:9][C:10]1[CH:11]=[C:12]2[C:17](=O)[O:16][C:14](=[O:15])[C:13]2=[CH:19][CH:20]=1.N1C=CC=CC=1.C(OC(=O)C)(=O)C>O.CC(N(C)C)=O>[I:1][C:2]1[CH:8]=[CH:7][C:5]([N:6]2[C:17](=[O:16])[C:12]3=[CH:11][C:10]([I:9])=[CH:20][CH:19]=[C:13]3[C:14]2=[O:15])=[CH:4][CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 1049PyridineHCID 7918Acetic AnhydrideHCID 108934-IodoanilineHCID 152633775-Iodo-2-benzofuran-1,3-dione

生成物 1

HCID 19737610HCID 19737610、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 31374
Dimethylacetamide
溶媒

反応条件

温度
70 °C

実験手順

##STR19## A 100 milliliter round-bottomed flask, equipped with stirrer, was charged with p-iodoaniline (10.95 grams, 0.05 mol) and dimethylacetamide (DMAc) (35 milliliters). 4-iodophthalic anhydride (13.6 grams, 0.05 mol) was added slowly over 10 minutes. The reaction mixture was heated with stirring to a temperature of about 70° C. Pyridine (19.45 grams, 0.25 mol) was added, the reaction mixture was stirred for 15 minutes, then acetic anhydride (11.12 grams, 0.11 mol) was added dropwise over 20 minutes. The reaction mixture was stirred at 70° C. overnight. The reaction mixture was poured into water, producing a white solid product, which was collected by filtration, triturated with methanol (300 milliliters) and dried under vacuum at 60° C. overnight. Melting point, as determined by DSC was 235° C. Combustion analysis was: calculated: C=35.40, H=1.49, N=2.95; measured: C=35.47, H=1.59, N=2.94. Proton NMR was consistent with the above general structure.

後処理

  1. custom##STR19## A 100 milliliter round-bottomed flask, equipped with stirrer
  2. temperatureThe reaction mixture was heated
  3. stirringthe reaction mixture was stirred for 15 minutes
  4. stirringThe reaction mixture was stirred at 70° C. overnight
  5. customproducing a white solid product, which
  6. filtrationwas collected by filtration
  7. customtriturated with methanol (300 milliliters)
  8. customdried under vacuum at 60° C. overnight
  9. customwas 235° C

出典と根拠

ORDレコード
ord-9ff793e2ac0b4ffcb65128a1e6821e0d
出典データセット
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05241038

反応ノート

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