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Dimethylamine → HCID 59511157, 화합물

HRID 1157824
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HRID 1157824 반응식
Cl[C:2]1[N:7]=[N:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[C:4]([N:14]2[CH2:19][CH2:18][N:17]([C:20]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[O:21])[CH2:16][CH2:15]2)[CH:3]=1.[CH3:28][NH:29][CH3:30]>CO.C1COCC1>[CH3:28][N:29]([CH3:30])[C:2]1[N:7]=[N:6][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[C:4]([N:14]2[CH2:19][CH2:18][N:17]([C:20]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[O:21])[CH2:16][CH2:15]2)[CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 674DimethylamineHCID 59511172HCID 59511172, 화합물

생성물 1

HCID 59511157HCID 59511157, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

To (4-(6-chloro-3-phenylpyridazin-4-yl)piperazin-1-yl)(phenyl)methanone (1 g) dissolved in methanol (40 ml), and dimethyl amine in THF (10 ml) was added under nitrogen atmosphere and the reaction mixture was heated to 60° C. for 18 hrs. The progress of reaction was monitored by TLC. After consumption of starting material, reaction mixture was cooled to room temperature and neutralized with solid sodium bicarbonate. The mixture was extracted with dichloromethane (3×10 ml). The combined organic layer was dried over anhydrous sodium sulphate and concentrated to afford (4-(6-(dimethylamino)-3-phenylpyridazin-4-yl)piperazin-1-yl)(phenyl)methanone as yellow liquid.

후처리

  1. customThe progress of reaction
  2. customAfter consumption of starting material, reaction mixture
  3. temperaturewas cooled to room temperature and neutralized with solid sodium bicarbonate
  4. extractionThe mixture was extracted with dichloromethane (3×10 ml)
  5. dry with materialThe combined organic layer was dried over anhydrous sodium sulphate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-9f73a8b371f94db3a6a0a2eeed66c6b4
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07807676B2

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