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

HRID 1900680노트

반응식

HRID 1900680 반응식
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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-bb9c7a4276a34320a7d4db9437819820
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05576322

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