Potassium Cyanide → 2-(4-((2-Amino-4-methyl-6-(pentylamino)pyrimidin-5-yl)methyl)-3-fluorophenyl)acetonitrile

HRID 2387819ノート

反応式

HRID 2387819 の反応式
[C-:1]#[N:2].[K+].Cl[CH2:5][C:6]1[CH:26]=[CH:25][C:9]([CH2:10][C:11]2[C:12]([NH:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[N:13][C:14]([NH2:18])=[N:15][C:16]=2[CH3:17])=[C:8]([F:27])[CH:7]=1>CS(C)=O.CN(C=O)C.CCOC(C)=O>[NH2:18][C:14]1[N:15]=[C:16]([CH3:17])[C:11]([CH2:10][C:9]2[CH:25]=[CH:26][C:6]([CH2:5][C:1]#[N:2])=[CH:7][C:8]=2[F:27])=[C:12]([NH:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])[N:13]=1

参加物

6

反応物 2

HCID 9032Potassium CyanideHCID 689525035-(4-(Chloromethyl)-2-fluorobenzyl)-6-methyl-N4-pentylpyrimidine-2,4-diamine

生成物 1

HCID 684148972-(4-((2-Amino-4-methyl-6-(pentylamino)pyrimidin-5-yl)methyl)-3-fluorophenyl)acetonitrile収率 64.1%

試薬・触媒・溶媒 3

HCID 679Dimethyl Sulfoxide溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Potassium cyanide (0.473 g) was added to a stirred solution of the product from step (vi) (0.85 g) in DMSO (10 mL) and DMF (10 mL). The mixture was stirred at rt for 15 h, diluted with EtOAc, washed with saturated NaHCO3 solution, saturated brine dried, filtered and evaporated. The crude product was purified by chromatography eluting with 0 to 5% MeOH in DCM to afford the subtitle compound as a yellow solid 0.530 g.

後処理

  1. washwashed with saturated NaHCO3 solution, saturated brine
  2. customdried
  3. filtrationfiltered
  4. customevaporated
  5. customThe crude product was purified by chromatography
  6. washeluting with 0 to 5% MeOH in DCM

出典と根拠

ORDレコード
ord-e9256073d2e24bd4bbeee9856ec2140d
出典データセット
uspto-grants-2012_09
特許番号
US08268990B2

反応ノート

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