Methanol → 2-Methyl-1-propyl-1,3-benzodiazole-5-carboxylic acid

HRID 74261ノート

反応式

HRID 74261 の反応式
CO.[NH2:3][C:4]1[CH:5]=[C:6]([CH:10]=[CH:11][C:12]=1[NH:13][CH2:14][CH2:15][CH3:16])[C:7]([OH:9])=[O:8].Cl.[C:18](=N)(OC)[CH3:19]>C(OCC)C>[CH3:18][C:19]1[N:13]([CH2:14][CH2:15][CH3:16])[C:12]2[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][C:4]=2[N:3]=1

参加物

5

反応物 3

HCID 887MethanolHCID 10313100Ethanimidic acid, methyl ester, hydrochloride (1:1)HCID 115864403-Amino-4-(propylamino)benzoic acid

生成物 1

HCID 202988562-Methyl-1-propyl-1,3-benzodiazole-5-carboxylic acid収率 116.5%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

To a methanol (17 mL) solution of 3-amino-4-n-propylaminobenzoic acid (see Working Example 82-2) (1.68 g, 8.65 mmol) was added methyl acetimidate hydrochloride (1.14 g, 10.4 mmol), and this was heated to reflux for 4 hours. After the reaction was complete, this was cooled to room temperature, diethyl ether was added, and this was allowed to stand at room temperature for 10 minutes. The crystals obtained were filtered, and after being washed with diethyl ether, they were dried to yield the title compound (2.20 g, quant.).

後処理

  1. temperaturethis was heated
  2. temperatureto reflux for 4 hours
  3. customThe crystals obtained
  4. filtrationwere filtered
  5. washafter being washed with diethyl ether, they
  6. customwere dried

出典と根拠

ORDレコード
ord-3eb052daec9a47e6839ab79527356e8e
出典データセット
uspto-grants-2014_09
特許番号
US08829035B2

反応ノート

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