Water → HCID 178518275, 화합물

HRID 2236597

반응식

HRID 2236597 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 178518275HCID 178518275, 화합물수율 54.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-ff29bf10ff054da5b7ded7482f32fee4
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07713994B2

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