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Acetyl chloride → N-(4,6-Dichloropyrimidin-2-yl)acetamide

HRID 1730144
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HRID 1730144 반응식
C(O[C:5](=[O:7])[CH3:6])(=O)C.[NH2:8][C:9]1[N:14]=[C:13]([Cl:15])[CH:12]=[C:11]([Cl:16])[N:10]=1.C(Cl)(=O)C>>[C:5]([NH:8][C:9]1[N:14]=[C:13]([Cl:15])[CH:12]=[C:11]([Cl:16])[N:10]=1)(=[O:7])[CH3:6]
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참가 물질

4

반응물 3

HCID 6367Acetyl chlorideHCID 7918Acetic AnhydrideHCID 655222-Amino-4,6-dichloropyrimidine

생성물 1

HCID 12611964N-(4,6-Dichloropyrimidin-2-yl)acetamide

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온도
110 °C

실험 절차

A 250 ml. three necked flask was fitted with a mechanical stirrer and a reflux condenser with drying tube. The flask is charged with 50 ml. of acetic anhydride and 3.85 g of 2-amino-4,6-dichloropyrimidine (0.025 mole). Then, 10 ml. of acetyl chloride was added slowly and the mixture was heated to 110° C for 8 hours. The mixture was allowed to stand overnight at room temperature. The crystalline solid product which formed was filtered and washed with water and sodium bicarbonate solution. It was then recrystallized from 50% alcohol. There was obtained 3.8 g of 2-acetamido-4,6-dichloropyrimidine (PY-25) in the form of white crystals, melting point, 198°-200° C, yield, 74.5%.

후처리

  1. customthree necked flask was fitted with a mechanical stirrer and a reflux condenser
  2. customwith drying tube
  3. additionThe flask is charged with 50 ml
  4. customThe crystalline solid product which formed
  5. filtrationwas filtered
  6. washwashed with water and sodium bicarbonate solution
  7. customIt was then recrystallized from 50% alcohol

출처 및 근거

ORD 기록
ord-d9a1175b5f344b87b702f550625511ad
출처 데이터셋
uspto-grants-1976_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03991190

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