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Ammonium Hydroxide → HCID 16749041、化合物

HRID 1913302
ノート
印刷プレビュー

反応式

HRID 1913302 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 16749041HCID 16749041、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

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)+.

後処理

  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

出典と根拠

ORDレコード
ord-307d80b3888c44dea47883257fe0fc68
出典データセット
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08609692B2

反応ノート

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