Diisopropylethylamine → HCID 71187345、化合物

HRID 714401ノート

反応式

HRID 714401 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 71187345HCID 71187345、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-27dbaa507f8942b98806dacb9d7f3335
出典データセット
uspto-grants-2015_11
特許番号
US09187440B2

反応ノート

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