Water → 3-{7-[2-(4-Methyl-piperazin-1-yl)-pyridin-4-yl]-2-morpholin-4-yl-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidin-4-yl}-phenol

HRID 912099ノート

反応式

HRID 912099 の反応式
C[O:2][C:3]1[CH:4]=[C:5]([C:9]2[C:10]3[CH2:23][CH2:22][N:21]([C:24]4[CH:29]=[CH:28][N:27]=[C:26]([N:30]5[CH2:35][CH2:34][N:33]([CH3:36])[CH2:32][CH2:31]5)[CH:25]=4)[C:11]=3[N:12]=[C:13]([N:15]3[CH2:20][CH2:19][O:18][CH2:17][CH2:16]3)[N:14]=2)[CH:6]=[CH:7][CH:8]=1.C([S-])C.[Na+].O>CN(C)C=O>[CH3:36][N:33]1[CH2:34][CH2:35][N:30]([C:26]2[CH:25]=[C:24]([N:21]3[C:11]4[N:12]=[C:13]([N:15]5[CH2:16][CH2:17][O:18][CH2:19][CH2:20]5)[N:14]=[C:9]([C:5]5[CH:4]=[C:3]([OH:2])[CH:8]=[CH:7][CH:6]=5)[C:10]=4[CH2:23][CH2:22]3)[CH:29]=[CH:28][N:27]=2)[CH2:31][CH2:32]1

参加物

5

反応物 3

HCID 962WaterHCID 4459711Sodium ethanethiolateHCID 592449894-(3-Methoxy-phenyl)-7-[2-(4-methyl-piperazin-1-yl)-pyridin-4-yl]-2-morpholin-4-yl-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidine

生成物 1

HCID 248896073-{7-[2-(4-Methyl-piperazin-1-yl)-pyridin-4-yl]-2-morpholin-4-yl-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidin-4-yl}-phenol収率 17.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
150 °C

実験手順

4-(3-Methoxyphenyl)-7-[2-(4-methylpiperazin-1-yl)-pyridin-4-yl]-2-morpholin-4-yl-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidine (107 mg, 0.22 mmol) was heated at 150° C. in dimethylformamide (1 ml), and sodium ethanethiolate (275 mg, 3.3 mmol) was added at 15 minutes intervals in 3 portions. After heating at 150° C. for further 15 minutes followed by cooling, water (1 ml) was added, followed by washing with ethyl acetate (2 ml). After the aqueous layer was left overnight, the deposited precipitate was filtered off, and washed with water followed by drying, whereby a colorless solid was obtained (18 mg, 17.3% yield).

後処理

  1. temperatureby cooling
  2. washby washing with ethyl acetate (2 ml)
  3. filtrationthe deposited precipitate was filtered off
  4. washwashed with water
  5. customby drying
  6. customwhereby a colorless solid was obtained (18 mg, 17.3% yield)

出典と根拠

ORDレコード
ord-4fe883bd4a274716823750cd9e93f022
出典データセット
uspto-grants-2011_09
特許番号
US08022205B2

反応ノート

読み込み中…