Water → HCID 178518275、化合物

HRID 2236597

反応式

HRID 2236597 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][C:9]=1[OH:10])[CH2:5][NH2:6].C(N(CC)CC)C.[Br:18][C:19]1[CH:20]=[C:21]2[C:26](=[CH:27][CH:28]=1)[C:25](=[O:29])[NH:24][C:23](=[O:30])/[C:22]/2=[CH:31]/OC.O>CN(C)C=O>[Br:18][C:19]1[CH:20]=[C:21]2[C:26](=[CH:27][CH:28]=1)[C:25](=[O:29])[NH:24][C:23](=[O:30])/[C:22]/2=[CH:31]\[NH:6][CH2:5][C:4]1[CH:7]=[CH:8][C:9]([OH:10])=[C:2]([OH:1])[CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 91623DihydroxybenzylamineHCID 68692760(E)-6-bromo-4-(methoxymethylene)isoquinoline-1,3(2H,4H)-dione

生成物 1

HCID 178518275HCID 178518275、化合物収率 54.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

According to general procedure 1, an amount of 3, 4 dihydroxybenzylamine (0.596 g, 4.3 mmol), is dissolved in N,N-dimethylformamide (61 mL). 1.8 ml (12.9 mmol) of triethylamine is added followed by 1.21 g (4.3 mmol) of (4E)-6-bromo-4-(methoxymethylene)isoquinoline-1,3(2H,4H)-dione. After the mixture is stirred at room temperature for 30 min, water (5 mL) is added and the reaction mixture is stirred for 60 min. The precipitate is filtered and washed several times with anhydrous ether. The crude solid is then purified by high performance liquid chromatography to give 910 mg of a white solid. MS (ESI) m/z 389.7 (M+1).

後処理

  1. stirringthe reaction mixture is stirred for 60 min
  2. filtrationThe precipitate is filtered
  3. washwashed several times with anhydrous ether
  4. customThe crude solid is then purified by high performance liquid chromatography

出典と根拠

ORDレコード
ord-ff29bf10ff054da5b7ded7482f32fee4
出典データセット
uspto-grants-2010_05
特許番号
US07713994B2

関連ノート

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