Water → 2-(4-Hydroxypiperidino)-4-(3,4-methylenedioxybenzyl)amino-6-cyanoquinazoline

HRID 1900680ノート

反応式

HRID 1900680 の反応式
Cl[C:2]1[N:11]=[C:10]([NH:12][CH2:13][C:14]2[CH:19]=[CH:18][C:17]3[O:20][CH2:21][O:22][C:16]=3[CH:15]=2)[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:23]#[N:24])[CH:8]=2)[N:3]=1.[OH:25][CH:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1.CN(C)C=O.O>C(OCC)(=O)C>[OH:25][CH:26]1[CH2:31][CH2:30][N:29]([C:2]2[N:11]=[C:10]([NH:12][CH2:13][C:14]3[CH:19]=[CH:18][C:17]4[O:20][CH2:21][O:22][C:16]=4[CH:15]=3)[C:9]3[C:4](=[CH:5][CH:6]=[C:7]([C:23]#[N:24])[CH:8]=3)[N:3]=2)[CH2:28][CH2:27]1

参加物

6

反応物 4

HCID 962WaterHCID 6228DimethylformamideHCID 79341Piperidin-4-olHCID 211839842-Chloro-4-(3,4-methylenedioxybenzyl)amino-6-cyanoquinazoline

生成物 1

HCID 211839852-(4-Hydroxypiperidino)-4-(3,4-methylenedioxybenzyl)amino-6-cyanoquinazoline収率 35.9%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture comprising 339 mg of 2-chloro-4-(3,4-methylenedioxybenzyl)amino-6-cyanoquinazoline, 500 mg of 4-hydroxypiperidine and 20 ml of N,N-dimethylformamide was heated under reflux for 5 hours and poured into 50 ml of water, followed by the addition of 50 ml of ethyl acetate. The obtained mixture was filtered to remove insolubles. The organic layer of the filtrate was dried over magnesium sulfate and concentrated under a reduced pressure to give a crystalline residue. This residue was washed with chloroform to give 145 mg of the title compound.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 5 hours
  3. filtrationThe obtained mixture was filtered
  4. customto remove insolubles
  5. dry with materialThe organic layer of the filtrate was dried over magnesium sulfate
  6. concentrationconcentrated under a reduced pressure
  7. customto give a crystalline residue
  8. washThis residue was washed with chloroform

出典と根拠

ORDレコード
ord-bb9c7a4276a34320a7d4db9437819820
出典データセット
uspto-grants-1996_11
特許番号
US05576322

反応ノート

読み込み中…