Quinone → 7,8,9,10-Tetrahydro-11-(4-pyridyl)-6H-azepino[1,2-a]indole-3-ol

HRID 66823

반응식

HRID 66823 반응식
[N:1]1[CH:6]=[CH:5][C:4]([CH:7]=[C:8]2[CH2:14][CH2:13][CH2:12][CH2:11][CH2:10][NH:9]2)=[CH:3][CH:2]=1.[C:15]1(=O)[CH:20]=[CH:19][C:18](=[O:21])[CH:17]=[CH:16]1>C(Cl)(Cl)Cl>[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[C:15]3[C:16](=[CH:17][C:18]([OH:21])=[CH:19][CH:20]=3)[N:9]3[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][C:8]=23)=[CH:3][CH:2]=1

참가 물질

4

반응물 2

HCID 4650QuinoneHCID 705496552-(4-Picolinylidene)1,3,4,5,6,7-hexahydroazepine

생성물 1

HCID 205291797,8,9,10-Tetrahydro-11-(4-pyridyl)-6H-azepino[1,2-a]indole-3-ol

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

One hundred and forty-one grams (0.75 mole) of 2-(4-picolinylidene)1,3,4,5,6,7-hexahydroazepine were dissolved in 1000 ml of chloroform and mixed under ice cooling with a solution of 89 g (0.83 mole) of 1,4-benzoquinone in 1000 ml of chloroform added dropwise. After the mixture stood for 24 hours at room temperature, the precipitate formed was filtered, suspended in 500 ml of dimethylformamide, and then heated for two hours to 100° C. After cooling, the suspension was suction filtered and washed with dimethylformamide and acetone, whereby the pure 2-hydroxy-isomer was obtained.

후처리

  1. additionadded dropwise
  2. customthe precipitate formed
  3. filtrationwas filtered
  4. temperatureheated for two hours to 100° C
  5. temperatureAfter cooling
  6. filtrationfiltered
  7. washwashed with dimethylformamide and acetone, whereby the pure 2-hydroxy-isomer
  8. customwas obtained

출처 및 근거

ORD 기록
ord-a85841b2f3f94a06bf8c65be4734c04c
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04343811

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