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Acetic Acid → HCID 68467418、化合物

HRID 506176
ノート
印刷プレビュー

反応式

HRID 506176 の反応式
[CH:1]([C:3]1[CH:4]=[CH:5][C:6]2[S:10][C:9]([C:11]3[CH:12]=[N:13][CH:14]=[C:15]([C:18]=3[NH:19][C:20]3[CH:28]=[CH:27][CH:26]=[C:25]4[C:21]=3[CH:22]=[CH:23][NH:24]4)[C:16]#[N:17])=[CH:8][C:7]=2[CH:29]=1)=O.[CH3:30][NH:31][CH3:32].C(O)(=O)C.[BH-](OC(C)=O)(OC(C)=O)OC(C)=O.[Na+]>C1COCC1>[CH3:30][N:31]([CH2:1][C:3]1[CH:4]=[CH:5][C:6]2[S:10][C:9]([C:11]3[CH:12]=[N:13][CH:14]=[C:15]([C:18]=3[NH:19][C:20]3[CH:28]=[CH:27][CH:26]=[C:25]4[C:21]=3[CH:22]=[CH:23][NH:24]4)[C:16]#[N:17])=[CH:8][C:7]=2[CH:29]=1)[CH3:32]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 674Dimethylamine2 回HCID 5049666Sodium triacetoxyborohydrideHCID 86616831HCID 86616831、化合物

生成物 1

HCID 68467418HCID 68467418、化合物収率 65%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒
2 回

実験手順

To 5-(5-formyl-1-benzothien-2-yl)-4-(1H-indol-4-ylamino)nicotinonitrile 223 (166 mg, 0.38 mmol) in THF (7 mL) was added dimethylamine in THF (2.0 M, 0.58 mL, 1.15 mmol) followed by acetic acid (126 mg, 2.09 mmol). The resulting mixture was stirred at r.t. for 1 h and additional dimethylamine (1.2 mL, 2.30 mmol) was added. After stirring at r.t. for an additional hour, Na(OAc)3BH (242 mg, 1.15 mmol) was added. The reaction mixture was stirred at r.t. for 2 h and was partitioned between diluted HCl and EtOAc. The combined aqueous extracts were basified with aqueous NaHCO3 and extracted with EtOAc. The combined organics were dried over Na2SO4, concentrated and purified by flash column chromatography to give 115 mg (65%) of 5-{5-[(dimethylamino)methyl]-1-benzothien-2-yl}-4-(1H-indol-4-ylamino)nicotinonitrile 224 as a pale yellow solid. MS: 424.2 (M+H); HPLC retention time: 2.1 min.(a).

後処理

  1. stirringAfter stirring at r.t. for an additional hour
  2. stirringThe reaction mixture was stirred at r.t. for 2 h
  3. customwas partitioned between diluted HCl and EtOAc
  4. extractionextracted with EtOAc
  5. dry with materialThe combined organics were dried over Na2SO4
  6. concentrationconcentrated
  7. custompurified by flash column chromatography

出典と根拠

ORDレコード
ord-1f4f9017616b4df89f1f433e248de6fd
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07781591B2

反応ノート

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