23138-53-6 → Methyl 4-({[4-(4-isopropoxy-6-morpholin-4-yl-1,3,5-triazin-2-yl)phenyl]carbamoyl}amino)benzoate

HRID 536840ノート

反応式

HRID 536840 の反応式
[CH:1]([O:4][C:5]1[N:10]=[C:9]([N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[N:8]=[C:7]([C:17]2[CH:23]=[CH:22][C:20]([NH2:21])=[CH:19][CH:18]=2)[N:6]=1)([CH3:3])[CH3:2].[C:24]([C:28]1[CH:33]=[CH:32][C:31]([N:34]=[C:35]=[O:36])=[CH:30][CH:29]=1)([O:26][CH3:27])=[O:25]>C(N(CC)CC)C>[CH:1]([O:4][C:5]1[N:10]=[C:9]([N:11]2[CH2:16][CH2:15][O:14][CH2:13][CH2:12]2)[N:8]=[C:7]([C:17]2[CH:23]=[CH:22][C:20]([NH:21][C:35]([NH:34][C:31]3[CH:32]=[CH:33][C:28]([C:24]([O:26][CH3:27])=[O:25])=[CH:29][CH:30]=3)=[O:36])=[CH:19][CH:18]=2)[N:6]=1)([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 28045423138-53-6HCID 67021898HCID 67021898、化合物

生成物 1

HCID 44517287Methyl 4-({[4-(4-isopropoxy-6-morpholin-4-yl-1,3,5-triazin-2-yl)phenyl]carbamoyl}amino)benzoate

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

A mixture of 4-(4-isopropoxy-6-morpholino-1,3,5-triazin-2-yl)aniline (1.3 g, 4.1 mmol), triethylamine (2 ml) and 4-carbomethoxy-phenylisocyanate (1451 mg, 8.2 mmol) was stirred for 48 hours and quenched with water and washed well. The organic layer was dried and filtered. It was concentrated and purified by column chromatography by eluting it initially with 10% ethyl acetate:hexane and latter with 40% ethyl acetate:hexane. White solid; 600 mg, 30%; MS (ESI) m/z 492.5.

後処理

  1. customquenched with water
  2. washwashed well
  3. customThe organic layer was dried
  4. filtrationfiltered
  5. concentrationIt was concentrated
  6. custompurified by column chromatography
  7. washby eluting it initially with 10% ethyl acetate

出典と根拠

ORDレコード
ord-f313167c73e948988d637ce97f3c4591
出典データセット
uspto-grants-2014_10
特許番号
US08859542B2

反応ノート

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