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Sodium Hydroxide → HCID 59756561, 화합물

HRID 2405752
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HRID 2405752 반응식
P(Cl)(Cl)([Cl:3])=O.[NH2:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][C:16]=1[Cl:17])[C:13](=O)[NH:12][CH:11]=[CH:10]2.[OH-].[Na+]>>[Cl:3][C:13]1[C:14]2[C:9](=[CH:8][C:7]([NH2:6])=[C:16]([Cl:17])[CH:15]=2)[CH:10]=[CH:11][N:12]=1
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참가 물질

4

반응물 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 108780456-amino-7-chloro-2H-isoquinolin-1-one

생성물 1

HCID 59756561HCID 59756561, 화합물수율 55%

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온도
100 °C

실험 절차

To 20.0 mL (215 mmol) of phosphorous oxychloride, cooled to 0 C, was added 5.00 g (25.7 mmol) of 6-amino-7-chloro-2H-isoquinolin-1-one in portions. The mixture was heated to 100° C. for 3 h then cooled to room temperature and poured over ice. After all of the ice had melted the pH of the mixture was adjusted to slightly alkaline by the slow addition of a 10% aqueous NaOH solution. A yellow solid precipitated from solution and was collected by filtration, washed with water and dried over anhydrous Na2SO4 to provide 3.0 g (55%) of 1,7-dichloro-isoquinolin-6-ylamine. MS calc. for C9H7Cl2N2 [M+H]+: 214.08. Found: 213.23 and 215.23.

후처리

  1. temperaturethen cooled to room temperature
  2. additionpoured over ice
  3. customA yellow solid precipitated from solution
  4. filtrationwas collected by filtration
  5. washwashed with water
  6. dry with materialdried over anhydrous Na2SO4

출처 및 근거

ORD 기록
ord-7e9deb1825fc46aa984d99e17f66c362
출처 데이터셋
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08809326B2

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