Phosphoric Acid → HCID 20145026、化合物

HRID 1906017ノート

反応式

HRID 1906017 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH2:11][CH2:12][NH:13][C:14]([C:16]2[S:20][C:19]([NH:21]C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)=[N:18][C:17]=2[CH3:41])=O)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].OP(O)(O)=O>O>[NH2:21][C:19]1[S:20][C:16]([C:14]2[C:6]3[C:5](=[CH:4][C:3]([O:2][CH3:1])=[C:8]([O:9][CH3:10])[CH:7]=3)[CH2:11][CH2:12][N:13]=2)=[C:17]([CH3:41])[N:18]=1

参加物

4

反応物 2

HCID 1004Phosphoric AcidHCID 20144993HCID 20144993、化合物

生成物 1

HCID 20145026HCID 20145026、化合物収率 24.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

A mixture of N-[2-(3,4-dimethoxyphenyl)ethyl]-4-methyl-2-tritylamino-5-thiazolecarboxamide (5.0 g) and polyphospholic acid (116% as H3PO4, 50 g) was stirred at 100° C. for 10 hours. After the reaction mixture was cooled, water (250 ml) was added and stirred for 1 hour. After removal of insoluble materials by filtration, the filtrate was neutralized with sodium carbonate. From the aqueous solution was extracted the desired compound with chloroform, and the extract was dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was triturated in diisopropyl ether to afford 1-(2-amino-4-methylthiazol-5-yl)-6,7-dimethoxy-3,4-dihydroisoquinoline (0.67 g).

後処理

  1. temperatureAfter the reaction mixture was cooled
  2. stirringstirred for 1 hour
  3. customAfter removal of insoluble materials
  4. filtrationby filtration
  5. extractionFrom the aqueous solution was extracted the desired compound with chloroform
  6. dry with materialthe extract was dried over magnesium sulfate
  7. customThe solvent was evaporated under reduced pressure
  8. customthe residue was triturated in diisopropyl ether

出典と根拠

ORDレコード
ord-73cc14d2f4174adcaa1e35af2ba3d854
出典データセット
uspto-grants-1987_03
特許番号
US04649146

反応ノート

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