Diisopropylethylamine → HCID 71187345, 화합물

HRID 714401노트

반응식

HRID 714401 반응식
[Br:1][C:2]1[N:6]=[C:5](Cl)[S:4][N:3]=1.Cl.Cl.[CH3:10][O:11][C:12]1[CH:25]=[CH:24][C:15]([CH2:16][CH2:17][N:18]2[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)=[CH:14][CH:13]=1.CCN(C(C)C)C(C)C>CCO>[Br:1][C:2]1[N:6]=[C:5]([N:21]2[CH2:20][CH2:19][N:18]([CH2:17][CH2:16][C:15]3[CH:24]=[CH:25][C:12]([O:11][CH3:10])=[CH:13][CH:14]=3)[CH2:23][CH2:22]2)[S:4][N:3]=1

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 27250533-Bromo-5-chloro-1,2,4-thiadiazoleHCID 122357181-(4-Methoxyphenethyl)piperazine dihydrochloride

생성물 1

HCID 71187345HCID 71187345, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 3-bromo-5-chloro-1,2,4-thiadiazole (300 mg, 1.5 mmol), 1-(4-methoxyphenethyl)piperazine dihydrochloride (485 mg, 1.65 mmol) and DIPEA (641 mg, 867 μl, 4.96 mmol) in EtOH (10 mL) was stirred over night at ambient temperature. The mixture was concentrated in vacuo and the residue was purified by silica column chromatography eluting with a gradient formed from heptane and ethyl acetate to yield after evaporation of the product containing fractions 489 mg (85%) of the title compound as off-white solid. MS (m/e): 383.2 (MH+).

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue was purified by silica column chromatography
  3. washeluting with a gradient
  4. customformed from heptane and ethyl acetate
  5. customto yield
  6. customafter evaporation of the product
  7. additioncontaining fractions 489 mg (85%) of the title compound as off-white solid

출처 및 근거

ORD 기록
ord-27dbaa507f8942b98806dacb9d7f3335
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09187440B2

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