2-Amino-2-methyl-1,3-propanediol → 2-[[7-Amino-2-[[(2,3-difluorophenyl)methyl]thio]-4-pteridinyl]amino]-2-methyl-1,3-propanediol

HRID 1789939ノート

反応式

HRID 1789939 の反応式
[F:1][C:2]1[C:7]([F:8])=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:9][S:10][C:11]1[N:20]=[C:19](SCC2C=CC=C(F)C=2F)[C:18]2[C:13](=[N:14][C:15]([NH2:31])=[CH:16][N:17]=2)[N:12]=1.[NH2:32][C:33]([CH3:38])([CH2:36][OH:37])[CH2:34][OH:35]>CN1C=CN=C1>[NH2:31][C:15]1[N:14]=[C:13]2[C:18]([C:19]([NH:32][C:33]([CH3:38])([CH2:36][OH:37])[CH2:34][OH:35])=[N:20][C:11]([S:10][CH2:9][C:3]3[CH:4]=[CH:5][CH:6]=[C:7]([F:8])[C:2]=3[F:1])=[N:12]2)=[N:17][CH:16]=1

参加物

4

反応物 2

HCID 15312-Amino-2-methyl-1,3-propanediolHCID 220370392,4-Bis[[(2,3-difluorophenyl)methyl]thio]-7-pteridinamine

生成物 1

HCID 101583542-[[7-Amino-2-[[(2,3-difluorophenyl)methyl]thio]-4-pteridinyl]amino]-2-methyl-1,3-propanediol

試薬・触媒・溶媒 1

HCID 13901-Methylimidazole溶媒

実験手順

A solution of the product from example 1, step (c) (0.25 g) and 2-amino-2-methyl-1,3-propanediol (0.28 ml) in N-methylimidazole (1 ml) was heated in a microwave at 160° C. for 95 minutes. After cooling, the reaction mixture was partitioned between ethyl acetate and saturated aqueous ammonium chloride. The organic phase was dried over magnesium sulphate, filtered and evaporated to give a brown oil which was purified by silica gel flash column chromatography, eluting with 10:1 dichloromethane:methanol to give the title compound as a pale brown solid (0.031 g).

後処理

  1. temperatureAfter cooling
  2. customthe reaction mixture was partitioned between ethyl acetate and saturated aqueous ammonium chloride
  3. dry with materialThe organic phase was dried over magnesium sulphate
  4. filtrationfiltered
  5. customevaporated
  6. customto give a brown oil which
  7. customwas purified by silica gel flash column chromatography
  8. washeluting with 10:1 dichloromethane

出典と根拠

ORDレコード
ord-b1480fa09b40490e844336d04e3d4254
出典データセット
uspto-grants-2006_07
特許番号
US07071193B2

反応ノート

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