Methanol → 5-Amino-2-(2-(methylsulfonyl)ethyl)isoquinolin-1(2H)-one

HRID 1037784ノート

反応式

HRID 1037784 の反応式
[CH3:1][S:2]([CH2:5][CH2:6][N:7]1[CH:16]=[CH:15][C:14]2[C:9](=[CH:10][CH:11]=[CH:12][C:13]=2[N+:17]([O-])=O)[C:8]1=[O:20])(=[O:4])=[O:3].CO>>[NH2:17][C:13]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:14]=1[CH:15]=[CH:16][N:7]([CH2:6][CH2:5][S:2]([CH3:1])(=[O:4])=[O:3])[C:8]2=[O:20]

参加物

3

反応物 2

HCID 887MethanolHCID 595798122-(2-(Methylsulfonyl)ethyl)-5-nitroisoquinolin-1(2H)-one

生成物 1

HCID 595796075-Amino-2-(2-(methylsulfonyl)ethyl)isoquinolin-1(2H)-one

実験手順

Into a 250 ml round bottom flask was combined 2-(2-(methylsulfonyl)ethyl)-5-nitroisoquinolin-1(2H)-one (1.20 g, 0.00405 mol) Palladium/C (0.04 g, 0.0004 mol) and methanol (40 mL, 1 mol). The flask was evacuated and purged with hydrogen 3 times. The mixture was stirred at room temperature under hydrogen (1 atm) for three hours. The mixture was filtered over celite and the filtrate was reduced in vacuo. The mixture was purified by column chromatography using a Methanol:methylene chloride (0-10%) gradient. The combined pure fractions were reduced in vacuo to yield the title compound as an off white solid.

後処理

  1. customInto a 250 ml round bottom flask was combined
  2. customThe flask was evacuated
  3. custompurged with hydrogen 3 times
  4. filtrationThe mixture was filtered over celite
  5. customThe mixture was purified by column chromatography

出典と根拠

ORDレコード
ord-441c443a234d4a5fb3258bfa1dfe05c5
出典データセット
uspto-grants-2013_10
特許番号
US08546579B2

反応ノート

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