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Hydrochloric Acid → 4-(3-Amino-6-benzyloxy-7-methoxyquinoline-4-carbonyl)benzonitrile

HRID 2404230
ノート
印刷プレビュー

反応式

HRID 2404230 の反応式
[CH2:1]([O:8][C:9]1[CH:10]=[C:11]2[C:16](=[CH:17][C:18]=1[O:19][CH3:20])[N:15]=[CH:14][C:13]([N+:21]([O-])=O)=[C:12]2[C:24]([C:26]1[CH:33]=[CH:32][C:29]([C:30]#[N:31])=[CH:28][CH:27]=1)=[O:25])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl>CO.C(OCC)(=O)C.[Fe]>[NH2:21][C:13]1[CH:14]=[N:15][C:16]2[C:11]([C:12]=1[C:24]([C:26]1[CH:27]=[CH:28][C:29]([C:30]#[N:31])=[CH:32][CH:33]=1)=[O:25])=[CH:10][C:9]([O:8][CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)=[C:18]([O:19][CH3:20])[CH:17]=2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 313Hydrochloric AcidHCID 666328844-(6-Benzyloxy-7-methoxy-3-nitroquinoline-4-carbonyl)benzonitrile

生成物 1

HCID 666325404-(3-Amino-6-benzyloxy-7-methoxyquinoline-4-carbonyl)benzonitrile収率 70.9%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 887Methanol溶媒
HCID 8857
Ethyl Acetate
溶媒

反応条件

温度
66 °C

実験手順

4-(6-Benzyloxy-7-methoxy-3-nitroquinoline-4-carbonyl)benzonitrile (8.82 g, 20.07 mmol), iron powder (11.21 g, 200.7 mmol) and 2.0 M hydrochloric acid (22.76 ml) are suspended in methanol (455 ml) (stirrer motor) and heated at 66° C. for 18 h. When the reaction is complete (TLC (HPTLC) monitoring), the solid material is filtered off through kieselguhr with suction and rinsed with tetrahydrofuran (500 ml). The filtrate is evaporated to half its volume in vacuo. Semi-saturated NaCl solution (300 ml) is subsequently added, and the mixture is extracted twice with ethyl acetate (300 ml each time). The combined organic phases are dried over sodium sulfate, filtered with suction and evaporated to dryness in vacuo. The residue obtained is dissolved in ethyl acetate and filtered through a little flash silica gel. The filtrate is evaporated in vacuo, the residue is suspended in ethyl acetate (70 ml) and ethanol (20 ml), subsequently filtered off with suction and dried in a high vacuum, giving 4-(3-amino-6-benzyloxy-7-methoxyquinoline-4-carbonyl)benzonitrile (5.83 g, 14.23 mmol) as a solid having a melting point of 192.6° C. MS: 410.1 (M+H+), TLC (HPTLC): Rf=0.36 (ethyl acetate).

後処理

  1. filtrationthe solid material is filtered off through kieselguhr with suction
  2. washrinsed with tetrahydrofuran (500 ml)
  3. customThe filtrate is evaporated to half its volume in vacuo
  4. additionSemi-saturated NaCl solution (300 ml) is subsequently added
  5. extractionthe mixture is extracted twice with ethyl acetate (300 ml each time)
  6. dry with materialThe combined organic phases are dried over sodium sulfate
  7. filtrationfiltered with suction
  8. customevaporated to dryness in vacuo
  9. customThe residue obtained
  10. filtrationfiltered through a little flash silica gel
  11. customThe filtrate is evaporated in vacuo
  12. filtrationethanol (20 ml), subsequently filtered off with suction
  13. customdried in a high vacuum

出典と根拠

ORDレコード
ord-64eb0f1bf88d413282ac1e8d631a57b9
出典データセット
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08802712B2

反応ノート

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