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 912099노트

반응식

HRID 912099 반응식
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

참가 물질

5

반응물 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

생성물 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}-phenol수율 17.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
150 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-4fe883bd4a274716823750cd9e93f022
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022205B2

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