Potassium Hydroxide → HCID 20391041、化合物

HRID 426533

反応式

HRID 426533 の反応式
[OH:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][C:8]([OH:15])=[CH:9][CH:10]=3)[C:5](=[O:16])[C:4]=2[CH:3]=1.[ClH:17].[Cl:18][CH2:19][CH2:20][CH2:21][N:22]1[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1.[OH-].[K+]>C1(C)C=CC=CC=1.O>[ClH:18].[ClH:17].[N:22]1([CH2:21][CH2:20][CH2:19][O:1][C:2]2[CH:14]=[CH:13][C:12]3[C:11]4[C:6](=[CH:7][C:8]([O:15][CH2:19][CH2:20][CH2:21][N:22]5[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]5)=[CH:9][CH:10]=4)[C:5](=[O:16])[C:4]=3[CH:3]=2)[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1

参加物

6

反応物 3

HCID 14797Potassium HydroxideHCID 79624N-(3-chloropropyl)piperidine hydrochlorideHCID 43541812,7-Dihydroxyfluoren-9-one

生成物 1

HCID 20391041HCID 20391041、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

A mixture of 63.6 g (0.30 mole) of 2,7-dihydroxy-fluoren-9-one, 188 g (0.95 mole) of 1-(3-chloropropyl) piperidine hydrochloride, 132 g (2.0 mole) of 85% potassium hydroxide in 900 ml of toluene and 300 ml of water is refluxed with vigorous stirring for 20 hours. The layers are separated upon cooling and the organic layer is washed 3 times with water, once with a saturated solution of sodium chloride and dried over anhydrous magnesium sulfate. The mixture is filtered and the solvent removed in vacuo. The residue is taken up in isopropyl alcohol and acidified to Congo Red with ethereal hydrogen chloride. The solid which precipitates is filtered, recrystallized from a mixture of 3 parts isopropyl alcohol to 1 part methanol, and the 2,7-bis(3-piperidinopropoxy)fluoren-9-one dihydrochloride so prepared is dried at 100° C. for 24 hours under vacuum, m.p. 279.5°-80.5° C., λmaxH2O 270, and E1cm1% 1370.

後処理

  1. temperatureis refluxed
  2. customThe layers are separated
  3. temperatureupon cooling
  4. washthe organic layer is washed 3 times with water
  5. dry with materialonce with a saturated solution of sodium chloride and dried over anhydrous magnesium sulfate
  6. filtrationThe mixture is filtered
  7. customthe solvent removed in vacuo
  8. customThe solid which precipitates
  9. filtrationis filtered
  10. customrecrystallized from a mixture of 3 parts isopropyl alcohol to 1 part methanol
  11. customthe 2,7-bis(3-piperidinopropoxy)fluoren-9-one dihydrochloride so prepared
  12. customis dried at 100° C. for 24 hours under vacuum, m.p. 279.5°-80.5° C., λmaxH2O 270, and E1cm1% 1370

出典と根拠

ORDレコード
ord-360135aef7d54317bbf552753ebe0a2f
出典データセット
uspto-grants-1979_10
特許番号
US04169897

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