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Potassium Carbonate → 6-(6-Methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylmethyl)-3-vinyl-quinoline

HRID 655304
ノート
印刷プレビュー

反応式

HRID 655304 の反応式
Br[C:2]1[CH:3]=[N:4][C:5]2[C:10]([CH:11]=1)=[CH:9][C:8]([CH2:12][C:13]1[N:17]3[N:18]=[C:19]([CH3:22])[CH:20]=[CH:21][C:16]3=[N:15][N:14]=1)=[CH:7][CH:6]=2.[CH:23](B(O)O)=[CH2:24].C([O-])([O-])=O.[K+].[K+].O1CCOCC1>C1C=CC([PH+]([C]2[CH][CH][CH][CH]2)C2C=CC=CC=2)=CC=1.C1C=CC([PH+]([C]2[CH][CH][CH][CH]2)C2C=CC=CC=2)=CC=1.C(Cl)Cl.Cl[Pd]Cl.[Fe].O>[CH3:22][C:19]1[CH:20]=[CH:21][C:16]2[N:17]([C:13]([CH2:12][C:8]3[CH:9]=[C:10]4[C:5](=[CH:6][CH:7]=3)[N:4]=[CH:3][C:2]([CH:23]=[CH2:24])=[CH:11]4)=[N:14][N:15]=2)[N:18]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 11430Potassium CarbonateHCID 312751,4-DioxaneHCID 4683185Vinylboronic acidHCID 593202953-Bromo-6-(6-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylmethyl)-quinoline

生成物 1

HCID 249669426-(6-Methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylmethyl)-3-vinyl-quinoline収率 35%

試薬・触媒・溶媒 2

HCID 53485975
CID 53485975
触媒
HCID 962Water溶媒

実験手順

To a microwave vessel was added 3-bromo-6-(6-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylmethyl)-quinoline (500 mg, 1.41 mmol, 1 equiv), vinyl boronic acid (299 uL, 1.76 mmol, 1.25 equiv), K2CO3 (390 mg, 2.82 mmol, 2.0 equiv) followed by 1,4-dioxane (10 mL) and water (5 mL). The solution was degassed with nitrogen for 10 min and then dichloro[1,1′-bis(diphenylphosphino)ferrocene]palladium(II) dichloromethane adduct (51 mg, 0.07 mmol, 0.05 equiv) was added. The microwave vessel was capped and reacted in a microwave reactor at 130° C. for 30 min. The microwave vessel was cooled and then the mixture was extracted into dichloromethane and washed with water. The volatiles were removed in vacuo and the residue absorbed onto silica gel and purified by flash chromatography (SiO2, CH2Cl2:CH3OH 100:0-80:20) to obtain the title compound as a brown oil (35% yield). Analytical data presented in Table 1.

後処理

  1. customThe solution was degassed with nitrogen for 10 min
  2. customThe microwave vessel was capped
  3. customreacted in a microwave reactor at 130° C. for 30 min
  4. temperatureThe microwave vessel was cooled
  5. extractionthe mixture was extracted into dichloromethane
  6. washwashed with water
  7. customThe volatiles were removed in vacuo
  8. customthe residue absorbed onto silica gel
  9. custompurified by flash chromatography (SiO2, CH2Cl2:CH3OH 100:0-80:20)

出典と根拠

ORDレコード
ord-b796d5fdb4244f89a7e5df2305cfdf02
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08071581B2

反応ノート

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