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1-Methylpiperazine → 3-Fluoro-8-isopropyl-10-(4-methylpiperazino)-10,11-dihydrodibenzo(b,f)thiepin

HRID 1389286
ノート
印刷プレビュー

反応式

HRID 1389286 の反応式
FC1C=CC2CC(=O)C3C=C(C(C)C)C=CC=3SC=2C=1.CN1CCNCC1.C(O)(=O)/C=C\C(O)=O.C([O-])(=O)/C=C\C([O-])=O.[F:44][C:45]1[CH:46]=[CH:47][C:48]2[CH:54]=[C:53]([N:55]3[CH2:60][CH2:59][N:58]([CH3:61])[CH2:57][CH2:56]3)[C:52]3[CH:62]=[C:63]([CH:66]([CH3:68])[CH3:67])[CH:64]=[CH:65][C:51]=3[S:50][C:49]=2[CH:69]=1>C1C=CC=CC=1.C(O)C.[Ti](Cl)(Cl)(Cl)Cl.CCOCC.O>[F:44][C:45]1[CH:46]=[CH:47][C:48]2[CH2:54][CH:53]([N:55]3[CH2:56][CH2:57][N:58]([CH3:61])[CH2:59][CH2:60]3)[C:52]3[CH:62]=[C:63]([CH:66]([CH3:67])[CH3:68])[CH:64]=[CH:65][C:51]=3[S:50][C:49]=2[CH:69]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

11

反応物 5

HCID 531671-MethylpiperazineHCID 444266Maleic AcidHCID 8263943-fluoro-8-isopropyldibenzo(b,f)thiepin-10(11H)-oneHCID 30541753-Fluoro-8-isopropyl-10-(4-methylpiperazino)dibenzo(b,f)thiepinHCID 5288227Maleate(2-)

生成物 1

HCID 30541663-Fluoro-8-isopropyl-10-(4-methylpiperazino)-10,11-dihydrodibenzo(b,f)thiepin

試薬・触媒・溶媒 5

HCID 24193Titanium Tetrachloride触媒HCID 241Benzene溶媒3 回HCID 702Ethanol溶媒HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

A stirred solution of 8.0 g 3-fluoro-8-isopropyldibenzo(b,f)thiepin-10(11H)-one in 55 ml benzene is treated with a solution of 2.8 g titanium tetrachloride in 14 ml benzene added dropwise. 14 g of 1-methylpiperazine are then slowly added and the mixture refluxed for 16 hours. After cooling, it is decomposed with 80 ml water, added dropwise. 100 ml benzene are then added and the separated solid is filtered. The benzene layer of the filtrate is washed with water, dried with potassium carbonate and evaporated. There are obtained 9.2 g (89%) crude oily base which is neutralized with maleic acid in ethanol. Addition of ether separates the crystalline maleate of 3-fluoro-8-isopropyl-10-(4-methylpiperazino)dibenzo(b,f)thiepin melting at 183°-184° C. with decomposition (ethanol-ether).

後処理

  1. additionadded dropwise
  2. temperaturethe mixture refluxed for 16 hours
  3. temperatureAfter cooling
  4. additionadded dropwise
  5. filtrationthe separated solid is filtered
  6. washThe benzene layer of the filtrate is washed with water
  7. dry with materialdried with potassium carbonate
  8. customevaporated
  9. customThere are obtained 9.2 g (89%) crude oily base which

出典と根拠

ORDレコード
ord-9185e63d697445ea99dfb04f0363baca
出典データセット
uspto-grants-1981_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04243805

反応ノート

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