Hydrochloric Acid → HCID 66852213、化合物

HRID 1169637ノート

反応式

HRID 1169637 の反応式
C(N([CH2:6][CH3:7])CC)C.[C:8]([C:10]1[CH:15]=[CH:14][C:13]([CH2:16][CH:17]([CH3:19])[CH3:18])=[CH:12][CH:11]=1)#[CH:9].Cl.CN(C)[CH:23]=[O:24]>[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>[CH2:16]([C:13]1[CH:14]=[CH:15][C:10]([C:8]#[C:9][C:9]2[CH:8]=[C:10]3[C:15](=[CH:6][CH:7]=2)[C:23](=[O:24])[CH2:13][CH2:12][CH2:11]3)=[CH:11][CH:12]=1)[CH:17]([CH3:19])[CH3:18]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 6228Dimethylformamide2 回HCID 8471TriethylamineHCID 50540331-Ethynyl-4-(2-methylpropyl)benzene

生成物 1

HCID 66852213HCID 66852213、化合物

試薬・触媒・溶媒 1

HCID 11979704Tetrakis(triphenylphosphine)palladium触媒

実験手順

To cuprous iodide (48 mg), a solution of the compound (353 mg) prepared in Reference Example 06 in N,N-dimethylformamide (3 mL), triethylamine (279 μl) and a solution of 1-ethynyl-4-isobutylbenzene (158 mg) in N,N-dimethylformamide (5 mL) were added, followed by stirring at room temperature for 5 minutes. Next, tetrakis(triphenylphosphine) palladium (0) (58 mg) was added thereto, followed by stirring for 19 hours. After adding 1 N hydrochloric acid, the mixture was extracted with ethyl acetate. The organic layer was successively washed with 1 N hydrochloric acid, a saturated aqueous sodium hydrogencarbonate solution and a saturated aqueous sodium chloride solution, dried and concentrated. The residue thus obtained was purified by silica gel column chromatography (hexane:ethyl acetate=95:5) to thereby give the title compound (209 mg) having the following physical properties.

後処理

  1. stirringby stirring for 19 hours
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was successively washed with 1 N hydrochloric acid
  4. dry with materiala saturated aqueous sodium hydrogencarbonate solution and a saturated aqueous sodium chloride solution, dried
  5. concentrationconcentrated
  6. customThe residue thus obtained
  7. customwas purified by silica gel column chromatography (hexane:ethyl acetate=95:5)

出典と根拠

ORDレコード
ord-5bced749522a45628e2b881fac79a6a1
出典データセット
uspto-grants-2010_11
特許番号
US07825109B2

反応ノート

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