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Diisopropylethylamine → HCID 25054678, 화합물

HRID 1400089
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인쇄 미리보기

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HRID 1400089 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[N:6]=[N:5][C:4]=1[NH:13][CH:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1.[F:20][C:21]([F:31])([F:30])[C:22]1[CH:23]=[C:24]([CH:27]=[CH:28][CH:29]=1)[CH2:25]Br.C(N(C(C)C)CC)(C)C>C(#N)C.Cl.C(OCC)C>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]([F:12])([F:10])[F:11])[N:6]=[N:5][C:4]=1[NH:13][CH:14]1[CH2:19][CH2:18][N:17]([CH2:25][C:24]2[CH:27]=[CH:28][CH:29]=[C:22]([C:21]([F:20])([F:30])[F:31])[CH:23]=2)[CH2:16][CH2:15]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 81531DiisopropylethylamineHCID 1230611-(Bromomethyl)-3-(trifluoromethyl)benzeneHCID 59233384HCID 59233384, 화합물

생성물 1

HCID 25054678HCID 25054678, 화합물수율 109.6%

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 3283Diethyl Ether
용매
HCID 6342Acetonitrile용매

실험 절차

A mixture of (4-methoxy-6-trifluoromethyl-pyridazin-3-yl)-piperidin-4-yl-amine (D8) (0.10 g, 0.36 mmol), 3-trifluoromethyl-benzyl bromide (0.060 ml, 0.29 mmol) and diisopropylethylamine (0.138 ml, 0.79 mmol) in acetonitrile (2 ml) was stirred at room temperature for 16 h. After this period, the solvent was evaporated in vacuo and the crude product purified by short open column chromatography (silica gel; 3% ammonia in methanol (7M)/dichloromethane). The desired fractions were collected and evaporated in vacuo. The product thus obtained was dissolved in a solution 2M of hydrochloric acid in diethyl ether to yield the corresponding hydrochloride salt E4 (0.138 g, 88%) as a solid. C19H20F6N4O.HCl free base requires 434; Found 435 (MH+). Rt (Method 1): 4.73 min.

후처리

  1. waitAfter this period
  2. customthe solvent was evaporated in vacuo
  3. customthe crude product purified by short open column chromatography (silica gel; 3% ammonia in methanol (7M)/dichloromethane)
  4. customThe desired fractions were collected
  5. customevaporated in vacuo
  6. customThe product thus obtained

출처 및 근거

ORD 기록
ord-7c270af2c9c94b389ea2362407568e99
출처 데이터셋
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08906921B2

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