7-dimethylamino-6,7-dihydro [5H] benzocycloheptene → HCID 3046863、化合物

HRID 372542ノート

反応式

HRID 372542 の反応式
[CH3:1][N:2]([CH3:14])[CH:3]1[CH:9]=[CH:8][C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[CH2:5][CH2:4]1>C(O)C>[CH3:1][N:2]([CH3:14])[CH:3]1[CH2:9][CH2:8][C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[CH2:5][CH2:4]1

参加物

3

反応物 1

HCID 30468617-dimethylamino-6,7-dihydro [5H] benzocycloheptene

生成物 1

HCID 3046863HCID 3046863、化合物収率 36.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 11.2 g of 7-dimethylamino-6,7-dihydro [5H] benzocycloheptene, 800 ml of ethanol and 11.2 g carbon containing 10% of Pd (OH)2 was held under a hydrogen atmosphere for 30 minutes and when the theoretical amount of hydrogen had been absorbed, the mixture was filtered. The filtrate was evaporated to dryness and the residue was chromatographed over silica gel. Elution with an 8-2-1 ethyl acetate-benzene-triethylamine mixture yielded 4.1 g of 7-dimethylamino-6,7,8,9-tetrahydro [5H] benzocycloheptene.

後処理

  1. customwhen the theoretical amount of hydrogen had been absorbed
  2. filtrationthe mixture was filtered
  3. customThe filtrate was evaporated to dryness
  4. customthe residue was chromatographed over silica gel
  5. washElution with an 8-2-1 ethyl acetate-benzene-triethylamine mixture

出典と根拠

ORDレコード
ord-67190c1bc9fe4862a4af33c88bc1dd26
出典データセット
uspto-grants-1978_05
特許番号
US04091115

反応ノート

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