Dichloromethane → HCID 13560178, 화합물

HRID 637828노트

반응식

HRID 637828 반응식
N#N.CN(C)CCC[C:8]1[CH:13]=[CH:12][N:11]=[C:10]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]=1[NH2:21].[CH2:23]([N:25]([CH2:28][CH3:29])[CH2:26]C)C.[Cl:30][C:31]1[CH:39]=[CH:38][CH:37]=[CH:36][C:32]=1[C:33](Cl)=[O:34].[CH2:40](Cl)Cl>>[Cl:30][C:31]1[CH:39]=[CH:38][CH:37]=[CH:36][C:32]=1[C:33]([NH:21][C:9]1[C:10]([N:14]([CH2:40][CH2:29][CH2:28][N:25]([CH3:23])[CH3:26])[C:15]2[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=2)=[N:11][CH:12]=[CH:13][CH:8]=1)=[O:34]

참가 물질

5

반응물 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 691102-Chlorobenzoyl chlorideHCID 86740554HCID 86740554, 화합물

생성물 1

HCID 13560178HCID 13560178, 화합물수율 74%

실험 절차

To a stirred solution of 9 g (0.033 mole) of N2 -[3-(dimethylamino)propyl]-N2 -phenyl-2,3-pyridinediamine and 3.9 g (0.038 mole) triethylamine in 75 ml of dry methylene chloride was added dropwise with stirring at 15°-20° C., 6.4 g (0.037 mole) of 2-chlorobenzoyl chloride. After stirring overnight, the reaction mixture was washed with water. The methylene chloride layer was extracted twice with dilute sodium hydroxide solution, washed with water, dried over sodium sulfate and concentrated in vacuo. The residue was triturated in isopropyl ether to give 10 g (74%) of solid. A portion of this solid was recrystallized from isopropyl alcohol-isopropyl ether to give a cream colored solid, m.p. 90°-92° C.

후처리

  1. stirringAfter stirring overnight
  2. washthe reaction mixture was washed with water
  3. extractionThe methylene chloride layer was extracted twice with dilute sodium hydroxide solution
  4. washwashed with water
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated in vacuo
  7. customThe residue was triturated in isopropyl ether

출처 및 근거

ORD 기록
ord-d74acf394c104f1fb3e08e99e7171ced
출처 데이터셋
uspto-grants-1985_12
특허 번호
US04558132

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