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Pentylamine → 6-Methyl-N4-pentyl-5-(4-((tetrahydro-2H-pyran-2-yloxy)methyl)benzyl)pyrimidine-2,4-diamine

HRID 1617188
ノート
印刷プレビュー

反応式

HRID 1617188 の反応式
CC1C=C(C)C=C(C)C=1S(O[C:14]1[C:19]([CH2:20][C:21]2[CH:26]=[CH:25][C:24]([CH2:27][O:28][CH:29]3[CH2:34][CH2:33][CH2:32][CH2:31][O:30]3)=[CH:23][CH:22]=2)=[C:18]([CH3:35])[N:17]=[C:16]([NH2:36])[N:15]=1)(=O)=O.[CH2:37]([NH2:42])[CH2:38][CH2:39][CH2:40][CH3:41]>C(O)CCC>[CH3:35][C:18]1[N:17]=[C:16]([NH2:36])[N:15]=[C:14]([NH:42][CH2:37][CH2:38][CH2:39][CH2:40][CH3:41])[C:19]=1[CH2:20][C:21]1[CH:22]=[CH:23][C:24]([CH2:27][O:28][CH:29]2[CH2:34][CH2:33][CH2:32][CH2:31][O:30]2)=[CH:25][CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 8060PentylamineHCID 866768952-Amino-6-methyl-5-(4-((tetrahydro-2H-pyran-2-yloxy)methyl)benzyl)pyrimidin-4-yl 2,4,6-trimethylbenzenesulfonate

生成物 1

HCID 684154226-Methyl-N4-pentyl-5-(4-((tetrahydro-2H-pyran-2-yloxy)methyl)benzyl)pyrimidine-2,4-diamine

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

A mixture of the product from step (iii) (6.49 g) and n-pentylamine (7.34 ml) in 1-butanol was heated under reflux for 24 h. The solvent was evaporated and the residue partitioned between EtOAc and water. The organics were separated, dried and evaporated under reduced pressure. The residue was purified by column chromatography eluting with 8% MeOH/DCM to afford the subtitle compound, 3.4 g.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 24 h
  3. customThe solvent was evaporated
  4. customthe residue partitioned between EtOAc and water
  5. customThe organics were separated
  6. customdried
  7. customevaporated under reduced pressure
  8. customThe residue was purified by column chromatography
  9. washeluting with 8% MeOH/DCM

出典と根拠

ORDレコード
ord-749af9b865034e809959c7f94fb35932
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08765939B2

反応ノート

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