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Methylamine → HCID 178485847, 화합물

HRID 1408424
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HRID 1408424 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:12]=[CH:11][NH:10][N:9]=2)=[CH:4][C:3]=1[CH2:13][NH2:14].C([C:22]1[NH:23][CH:24]=CN=1)(C1NC=CN=1)=O.CN.C1C[O:32]CC1>ClCCl>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:12]=[CH:11][NH:10][N:9]=2)=[CH:4][C:3]=1[CH2:13][NH:14][C:24]([NH:23][CH3:22])=[O:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6329MethylamineHCID 8028Tetrahydrofuran2회HCID 5250894Bis-(1H-imidazol-2-YL)-methanoneHCID 178509482HCID 178509482, 화합물

생성물 1

HCID 178485847HCID 178485847, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 2-chloro-5-(1H-pyrazol-3-yl)benzenemethanamine (i.e. the product of Step C of Synthesis Example 4) (2.4 g, 11.6 mmol) in THF (12 mL) and dichloromethane (12 mL) at 10° C. was added carbonyl diimidazole (2.8 g, 17.3 mmol). The reaction mixture was stirred at ambient temperature for 30 minutes and then cooled to 0° C. A solution of methylamine in THF (2 M, 12.0 mL, 24 mmol) was added, and the reaction mixture was stirred at ambient temperature for 15 h. The reaction mixture was then diluted with dichloromethane, washed with water and brine, concentrated and purified by preparative TLC (2% methanol in chloroform as eluant) to provide the title product as a solid (1.0 g).

후처리

  1. temperaturecooled to 0° C
  2. stirringthe reaction mixture was stirred at ambient temperature for 15 h
  3. washwashed with water and brine
  4. concentrationconcentrated
  5. custompurified by preparative TLC (2% methanol in chloroform as eluant)

출처 및 근거

ORD 기록
ord-1e2a5676f5774b93b10c40b6f9f39898
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08921360B2

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