4-(4-Acetylaminophenyl)-1,2-Dihydro-1-Methyl-2-Ethylcarbamoyl-6-Methylthiophthalazine → HCID 9841541、化合物

HRID 48179ノート

反応式

HRID 48179 の反応式
C([NH:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[C:18]([S:21][CH3:22])[CH:19]=3)[CH:14]([CH3:23])[N:13]([C:24](=[O:28])[NH:25][CH2:26][CH3:27])[N:12]=2)=[CH:7][CH:6]=1)(=O)C>CO.[OH-].[Na+].O>[NH2:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[C:18]([S:21][CH3:22])[CH:19]=3)[CH:14]([CH3:23])[N:13]([C:24](=[O:28])[NH:25][CH2:26][CH3:27])[N:12]=2)=[CH:7][CH:6]=1

参加物

5

反応物 1

HCID 129861734-(4-Acetylaminophenyl)-1,2-Dihydro-1-Methyl-2-Ethylcarbamoyl-6-Methylthiophthalazine

生成物 1

HCID 9841541HCID 9841541、化合物収率 87%

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

The solution of acetyl amide 9 in methanol and NaOH (2 N) was refluxing until there is no more starting material left monitored by TLC. The solution was diluted with water, and extracted with DCM three times. Removal of the solvent afforded the crude product, which was purified by using a silica gel column, gave the desired products 12 (Yield: 87%). 1HNMR (CDCl3): 7.45 (d, J=8.6 Hz, 2H), 7.35-7.25 (m, 4H), 6.78 (d, J=8.6 Hz, 2H), 6.53 (br, 1H), 5.60 (q, J=13.2 Hz, 1H), 3.42 (m, 2H), 2.40 (s, 3H), 1.22 (m, 6H).

後処理

  1. waitleft
  2. extractionextracted with DCM three times
  3. customRemoval of the solvent
  4. customafforded the crude product, which
  5. customwas purified

出典と根拠

ORDレコード
ord-dac157113b8b4855a374a0ee0f45e116
出典データセット
uspto-grants-2004_03
特許番号
US06703390B2

反応ノート

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