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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Pyridine → HCID 19737610, 화합물

HRID 2255650
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HRID 2255650 반응식
[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
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

HCID 19737610HCID 19737610, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 31374
Dimethylacetamide
용매

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온도
70 °C

실험 절차

##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.

후처리

  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

출처 및 근거

ORD 기록
ord-9ff793e2ac0b4ffcb65128a1e6821e0d
출처 데이터셋
uspto-grants-1993_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05241038

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