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Ammonium Hydroxide → HCID 16749041, 화합물

HRID 1911287
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HRID 1911287 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[C:3]([NH:11][C:12](=[O:14])[CH3:13])[N:2]=1.[N+:15]([O-])([O-:17])=[O:16].[K+].[NH4+].[OH-]>OS(O)(=O)=O>[N+:15]([C:6]1[CH:7]=[CH:8][CH:9]=[C:10]2[C:5]=1[CH:4]=[C:3]([NH:11][C:12](=[O:14])[CH3:13])[N:2]=[CH:1]2)([O-:17])=[O:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14923Ammonium HydroxideHCID 24434Potassium NitrateHCID 12366594N-(Isoquinolin-3-yl)acetamide

생성물 1

HCID 16749041HCID 16749041, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

A solution of N-(isoquinolin-3-yl)acetamide (3.89 g, 20.9 mmol) in concentrated H2SO4 (40 mL) was cooled to 0° C. and solid potassium nitrate (2.53 g, 25.1 mmol) was added slowly in portions over 10 min. After stiffing for 1 h at 0° C., the reaction mixture was poured over ice (50 g), and neutralized with concentrated NH4OH solution. The resulting yellow solid was collected by vacuum filtration, washed with water, and dried in the vacuum oven at ambient temperature for 48 hours. This material was triturated with 1:1 CH3OH—CH2Cl2, collected by filtration, washed with CH2Cl2, and dried under vacuum. This provided 4.14 g of the title compound as a yellow solid in approximately 60% purity. MS (ESI+) m/z 232 (M+H)+.

후처리

  1. filtrationThe resulting yellow solid was collected by vacuum filtration
  2. washwashed with water
  3. customdried in the vacuum oven at ambient temperature for 48 hours
  4. customThis material was triturated with 1:1 CH3OH—CH2Cl2
  5. filtrationcollected by filtration
  6. washwashed with CH2Cl2
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-5047e92fa05c44beb2628e2f6cc0c392
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08604053B2

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