Triethylamine → N-(4-Bromoisoquinolin-8-yl)nicotinamide

HRID 1454936ノート

反応式

HRID 1454936 の反応式
Cl.[C:2](Cl)(=[O:9])[C:3]1[CH:8]=[CH:7][CH:6]=[N:5][CH:4]=1.C(N(CC)CC)C.[NH2:18][C:19]1[CH:20]=[CH:21][CH:22]=[C:23]2[C:28]=1[CH:27]=[N:26][CH:25]=[C:24]2[Br:29]>C1COCC1.CCOC(C)=O>[Br:29][C:24]1[C:23]2[C:28](=[C:19]([NH:18][C:2](=[O:9])[C:3]3[CH:8]=[CH:7][CH:6]=[N:5][CH:4]=3)[CH:20]=[CH:21][CH:22]=2)[CH:27]=[N:26][CH:25]=1

参加物

6

反応物 3

HCID 8471TriethylamineHCID 884383-Pyridinecarbonyl chloride, hydrochloride (1:1)HCID 4597724-Bromoisoquinolin-8-amine2 回

生成物 1

HCID 20580764N-(4-Bromoisoquinolin-8-yl)nicotinamide

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Nicotinoyl chloride hydrochloride (356 mg, 2 mmol) and triethylamine (558 μl, 2 mmol) are added to a solution of 8-amino-4-bromoisoquinoline (intermediate 23.2, 446 mg, 0.90 mmol) in anhydrous THF (25 ml). The reaction mixture is stirred overnight, diluted with AcOEt (200 ml) and washed twice with 1N NaOH (100 ml) and then the organic phase is dried over Na2SO4 and evaporated under vacuum. The residue is purified on silica gel, eluting with AcOEt.

後処理

  1. washwashed twice with 1N NaOH (100 ml)
  2. dry with materialthe organic phase is dried over Na2SO4
  3. customevaporated under vacuum
  4. customThe residue is purified on silica gel
  5. washeluting with AcOEt

出典と根拠

ORDレコード
ord-fc6380d33f424aff843c7a9fb354ed08
出典データセット
uspto-grants-2009_01
特許番号
US07482342B2

反応ノート

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