2-Dimethylaminopyridine → (3-methoxy-phenyl)-carbamic acid 3-{4-[N'-(3-methyl-benzylidene)-hydrazino]-6-morpholin-4-yl-pyrimidin-2-yl}-propyl ester

HRID 252978

反応式

HRID 252978 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH:24]=[CH:25][CH:26]=1)[CH:5]=[N:6][NH:7][C:8]1[CH:13]=[C:12]([N:14]2[CH2:19][CH2:18][O:17][CH2:16][CH2:15]2)[N:11]=[C:10]([CH2:20][CH2:21][CH2:22][OH:23])[N:9]=1.[CH3:27][O:28][C:29]1[CH:30]=[C:31]([N:35]=[C:36]=[O:37])[CH:32]=[CH:33][CH:34]=1.CN(C1C=CC=CN=1)C>C(#N)C>[CH3:1][C:2]1[CH:3]=[C:4]([CH:24]=[CH:25][CH:26]=1)[CH:5]=[N:6][NH:7][C:8]1[CH:13]=[C:12]([N:14]2[CH2:19][CH2:18][O:17][CH2:16][CH2:15]2)[N:11]=[C:10]([CH2:20][CH2:21][CH2:22][O:23][C:36](=[O:37])[NH:35][C:31]2[CH:32]=[CH:33][CH:34]=[C:29]([O:28][CH3:27])[CH:30]=2)[N:9]=1

参加物

5

反応物 3

HCID 218852-DimethylaminopyridineHCID 878433-Methoxyphenyl isocyanateHCID 668406793-{4-[N'-(3-methyl-benzylidene)-hydrazino]-6-morpholin-4-yl-pyrimidin-2-yl}-propan-1-ol

生成物 1

HCID 66841255(3-methoxy-phenyl)-carbamic acid 3-{4-[N'-(3-methyl-benzylidene)-hydrazino]-6-morpholin-4-yl-pyrimidin-2-yl}-propyl ester

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
60 °C

実験手順

S5; 3-{4-[N′-(3-methyl-benzylidene)-hydrazino]-6-morpholin-4-yl-pyrimidin-2-yl}-propan-1-ol (355 mg, 1 mmol) was dissolved in acetonitrile (4 mL). To the mixture was added m-methoxyphenylisocyanate (149 mg., 1 mmol) and a catalytic amount of dimethylaminopyridine. The reaction was stirred at 60° C. for 16 hours. The reaction was then cooled to 4° C., and the precipitate was filtered, washed with acetonitrile (1 mL) and dried to give Compound 1, (3-methoxy-phenyl)-carbamic acid 3-{4-[N′-(3-methyl-benzylidene)-hydrazino]-6-morpholin-4-yl-pyrimidin-2-yl}-propyl ester.

後処理

  1. temperatureThe reaction was then cooled to 4° C.
  2. filtrationthe precipitate was filtered
  3. washwashed with acetonitrile (1 mL)
  4. customdried

出典と根拠

ORDレコード
ord-82d6c132e0e44fc6b47f970f7b5632cb
出典データセット
uspto-grants-2011_01
特許番号
US07872005B2

関連ノート

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