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1-Bromo-4-fluorobenzene → 1-[3-(6-Fluoro-1,2-benzisoxazol-3-yl)propyl]-4-(4-fluorophenyl)-4-hydroxypiperidine

HRID 434404
ノート
印刷プレビュー

反応式

HRID 434404 の反応式
[Mg].Br[C:3]1[CH:8]=[CH:7][C:6]([F:9])=[CH:5][CH:4]=1.[F:10][C:11]1[CH:29]=[CH:28][C:14]2[C:15]([CH2:18][CH2:19][CH2:20][N:21]3[CH2:26][CH2:25][C:24](=[O:27])[CH2:23][CH2:22]3)=[N:16][O:17][C:13]=2[CH:12]=1.[Cl-].[NH4+]>BrC(Br)C.CCOCC.O1CCCC1>[F:10][C:11]1[CH:29]=[CH:28][C:14]2[C:15]([CH2:18][CH2:19][CH2:20][N:21]3[CH2:22][CH2:23][C:24]([C:3]4[CH:8]=[CH:7][C:6]([F:9])=[CH:5][CH:4]=4)([OH:27])[CH2:25][CH2:26]3)=[N:16][O:17][C:13]=2[CH:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 99931-Bromo-4-fluorobenzeneHCID 25517Ammonium ChlorideHCID 5462224MagnesiumHCID 132078191-[3-(6-Fluoro-1,2-benzisoxazol-3-yl)propyl]-4-piperidone

生成物 1

HCID 132078221-[3-(6-Fluoro-1,2-benzisoxazol-3-yl)propyl]-4-(4-fluorophenyl)-4-hydroxypiperidine収率 54%

試薬・触媒・溶媒 3

HCID 11201
1,1-Dibromoethane
触媒
HCID 3283Diethyl Ether溶媒3 回
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a suspension of 1.1 g of magnesium shavings and a few drops of dibromoethane in 30 ml of ether was added a solution of 7.9 g of p-bromofluorobenzene in 20 ml of ether at a rate to maintain reflux of the mixture. After the addition was complete, the mixture was slowly diluted with 30 ml of tetrahydrofuran and then a solution of 5 g of 1-[3-(6-fluoro-1,2-benzisoxazol-3-yl)propyl]-4-piperidone in 30 ml of tetrahydrofuran was slowly added. After one hr, the mixture was diluted with ether, poured into 400 ml of saturated ammonium chloride solution and extracted with ether. The organic extracts were washed with water (2×), saturated sodium chloride solution and dried over anhydrous magnesium sulfate, filtered and concentrated. The residue was recrystallized from hexanes/ether to give 3.6 g (54%) of product, mp 100°-101° C.

後処理

  1. temperatureto maintain
  2. temperaturereflux of the mixture
  3. additionAfter the addition
  4. extractionextracted with ether
  5. washThe organic extracts were washed with water (2×), saturated sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customThe residue was recrystallized from hexanes/ether

出典と根拠

ORDレコード
ord-971e61a003a8480681996ee90ff84b71
出典データセット
uspto-grants-1983_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04396770

反応ノート

読み込み中…

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