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Triethylamine → HCID 12907207, 화합물

HRID 1462285
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HRID 1462285 반응식
[C:1]([C:3]1[C:8]([C:9]#[N:10])=[N:7][C:6](O)=[C:5]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([Cl:18])[CH:13]=2)[N:4]=1)#[N:2].P(Cl)(Cl)([Cl:21])=O.C(N(CC)CC)C>>[C:1]([C:3]1[C:8]([C:9]#[N:10])=[N:7][C:6]([Cl:21])=[C:5]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([Cl:18])[CH:13]=2)[N:4]=1)#[N:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 8471TriethylamineHCID 24813Phosphorus oxychlorideHCID 178510650HCID 178510650, 화합물

생성물 1

HCID 12907207HCID 12907207, 화합물수율 84%

실험 절차

2,3-Dicyano-5-hydroxy-6-(m-chlorophenyl)pyrazine (25.67 g; 0.10 mole) was put into 46.2 g (0.30 mole) of phosphorus oxychloride. The mixture was cooled to 0° to 5° C., and with stirring 10.1 g (0.1 mole) of triethylamine was added dropwise over the period of 30 minutes. After the addition, the mixture was refluxed for 3 hours. The reaction mixture was worked up in the same way as in Example 3. Petroleum ether (50 ml) was added to the resulting oily product, and the precipitate was collected by filtration. Recrystallization from carbon tetrachloride afforded 23.1 g (yield 83%) of 2,3-dicyano-5-chloro-6-(m-chlorophenyl)pyrazine.

후처리

  1. temperatureThe mixture was cooled to 0° to 5° C.
  2. additionwas added dropwise over the period of 30 minutes
  3. additionAfter the addition
  4. temperaturethe mixture was refluxed for 3 hours
  5. filtrationthe precipitate was collected by filtration
  6. customRecrystallization from carbon tetrachloride

출처 및 근거

ORD 기록
ord-6a29c36dab0f48739947fe264e926622
출처 데이터셋
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04460403

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