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

HRID 2181610노트

반응식

HRID 2181610 반응식
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

참가 물질

5

반응물 1

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

생성물 1

HCID 9841541HCID 9841541, 화합물수율 87%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 14798Sodium Hydroxide용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-62b2123549cd4420b123a55a9e50ab4e
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06894048B2

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