7-dimethylamino-6,7-dihydro [5H] benzocycloheptene → HCID 3046863, 화합물

HRID 372542노트

반응식

HRID 372542 반응식
[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

참가 물질

3

반응물 1

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

생성물 1

HCID 3046863HCID 3046863, 화합물수율 36.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-67190c1bc9fe4862a4af33c88bc1dd26
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04091115

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