Benzoic Acid → HCID 69822365、化合物

HRID 2228346

反応式

HRID 2228346 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[C:8](=O)[CH:7]([CH3:13])[CH2:6]2.[NH:14]1C[CH2:17][CH2:16][CH2:15]1.[C:19](O)(=[O:26])C1C=CC=CC=1.[OH2:28].[C:29]1([CH3:35])[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1>>[CH2:29]([CH:34]([CH2:33][CH2:32][CH2:31][CH3:30])[CH2:19][O:26][C:17](=[O:28])[C:16]([C:15]#[N:14])=[C:8]1[C:9]2[C:5](=[CH:4][C:3]([O:2][CH3:1])=[CH:11][CH:10]=2)[CH2:6][CH:7]1[CH3:13])[CH3:35]

参加物

6

反応物 5

HCID 243Benzoic AcidHCID 962WaterHCID 1140TolueneHCID 31268PyrrolidineHCID 122904905-Methoxy-2-methylindan-1-one

生成物 1

HCID 69822365HCID 69822365、化合物

実験手順

The above 2,3-dihydro-5-methoxy-2-methyl-1H-inden-1-one (5.2 g) was reacted with 5.9 g of 2-ethyl-hexyl cyano acetate in the presence of catalytic amounts of pyrrolidine and benzoic acid in 100 ml of toluene. The reaction mixture was refluxed for 30 hours with simultaneous separation of water. Then, the cold reaction mixture was washed with water, concentrated and chromatographed in toluene containing 2% of propanol through SiO2 to yield 2.6 g of a yellow liquid. UV 347 nm (ε=33′450), MS: 355(M+), 243 (100%), 226, 198.

後処理

  1. customThen, the cold reaction mixture
  2. washwas washed with water
  3. concentrationconcentrated
  4. customchromatographed in toluene containing 2% of propanol through SiO2

出典と根拠

ORDレコード
ord-2d7fa24983514ab1ab0f9e1ad6ea1384
出典データセット
uspto-grants-2002_07
特許番号
US06416746B1

関連ノート

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