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Phosphoric Acid → 3-[4-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-1-yl]heptanenitrile phosphate

HRID 1505481
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HRID 1505481 반응식
[N:1]1[C:6]2[NH:7][CH:8]=[CH:9][C:5]=2[C:4]([C:10]2[CH:11]=[N:12][N:13]([CH:15]([CH2:19][CH2:20][CH2:21][CH3:22])[CH2:16][C:17]#[N:18])[CH:14]=2)=[N:3][CH:2]=1.[P:23](=[O:27])([OH:26])([OH:25])[OH:24]>C(O)(C)C>[P:23]([OH:27])([OH:26])([OH:25])=[O:24].[N:1]1[C:6]2[NH:7][CH:8]=[CH:9][C:5]=2[C:4]([C:10]2[CH:11]=[N:12][N:13]([CH:15]([CH2:19][CH2:20][CH2:21][CH3:22])[CH2:16][C:17]#[N:18])[CH:14]=2)=[N:3][CH:2]=1
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HCID 1004Phosphoric AcidHCID 498192963-[4-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-1-yl]heptanenitrile

생성물 1

HCID 498192973-[4-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-1-yl]heptanenitrile phosphate수율 86.6%

시약·촉매·용매 1

HCID 3776Isopropanol용매2회

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온도
60 °C

실험 절차

To a solution of 3-[4-(7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-1-yl]heptanenitrile (0.363 g, 1.23 mmol) in isopropyl alcohol (8.0 mL) was added phosphoric acid (0.133 g, 1.36 mmol) in 1.0 mL isopropyl alcohol at 60° C. The mixture was heated at 60° C. for 1 hour, then cooled to room temperature. The precipitate was filtered off and air dried, rinsed with ethyl ether, and then air dried further to provide the desired phosphoric acid salt (418 mg, 86.5%). 1H NMR (DMSO-d6, 400 MHz) δ 12.10 (1H, s), 8.78 (1H, s), 8.66 (1H, s), 8.36 (1H, s), 7.58 (1H, m), 6.97 (1H, m), 4.71 (1H, m), 3.18 (1H, m), 3.17 (1H, m), 1.93 (1H, m), 1.82 (1H, m), 1.21 (3H, m), 0.95 (1H, m), 0.78 (3H, t, J=7.2 Hz) ppm.

후처리

  1. temperaturecooled to room temperature
  2. filtrationThe precipitate was filtered off
  3. customair dried
  4. washrinsed with ethyl ether
  5. customair dried further

출처 및 근거

ORD 기록
ord-9e8c122c0d34488cb6a9499c43e529e1
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09216984B2

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