Hydrochloric Acid → 7-[[(7R)-7-ethyl-8-isopropyl-5-methyl-6-oxo-7H-pteridin-2-yl]amino]-2,3-dihydrobenzofuran-4-carboxylic acid

HRID 2364720ノート

反応式

HRID 2364720 の反応式
Cl[C:2]1[N:11]=[CH:10][C:9]2[N:8]([CH3:12])[C:7](=[O:13])[C@@H:6]([CH2:14][CH3:15])[N:5]([CH:16]([CH3:18])[CH3:17])[C:4]=2[N:3]=1.[NH2:19][C:20]1[CH:21]=[CH:22][C:23]([C:29]([OH:31])=[O:30])=[C:24]2[C:28]=1[O:27][CH2:26][CH2:25]2.Cl>C(O)C.O>[CH2:14]([C@H:6]1[N:5]([CH:16]([CH3:18])[CH3:17])[C:4]2[N:3]=[C:2]([NH:19][C:20]3[CH:21]=[CH:22][C:23]([C:29]([OH:31])=[O:30])=[C:24]4[C:28]=3[O:27][CH2:26][CH2:25]4)[N:11]=[CH:10][C:9]=2[N:8]([CH3:12])[C:7]1=[O:13])[CH3:15]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 249683367-Amino-2,3-dihydrobenzofuran-4-carboxylic acidHCID 58405561(R)-2-Chloro-7-ethyl-8-isopropyl-5-methyl-6-oxo-5,6,7,8-tetrahydropyrimido[4,5-b]pyrazine

生成物 1

HCID 681080517-[[(7R)-7-ethyl-8-isopropyl-5-methyl-6-oxo-7H-pteridin-2-yl]amino]-2,3-dihydrobenzofuran-4-carboxylic acid収率 65.1%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

(7R)-2-Chloro-7-ethyl-8-isopropyl-5-methyl-7H-pteridin-6-one 22d (82 mg, 3.07 mmol) and 7-amino-2,3-dihydrobenzofuran-4-carboxylic acid 22e (500 mg, 2.80 mmol) were dissolved in 34 mL of the mixture solvent of ethanol and water (V/V=1:2.4) followed by the addition of 0.4 mL of concentrated hydrochloric acid. The reaction solution was heated to reflux for 15 hours and cooled down resulting in the formation of precipitate. The precipitate was filtered to obtain the title compound 7-[[(7R)-7-ethyl-8-isopropyl-5-methyl-6-oxo-7H-pteridin-2-yl]amino]-2,3-dihydrobenzofuran-4-carboxylic acid 22f (0.75 g, yield: 65.0%) as a white solid.

後処理

  1. temperatureThe reaction solution was heated
  2. temperatureto reflux for 15 hours
  3. temperaturecooled down
  4. customresulting in the formation of precipitate
  5. filtrationThe precipitate was filtered

出典と根拠

ORDレコード
ord-5f743e0094b84f57aefe9e06c179eb17
出典データセット
uspto-grants-2014_04
特許番号
US08691822B2

反応ノート

読み込み中…