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Nitrogen → 1-[7-[2-(1,3-dioxolan-2-yl)thiazol-4-yl]-4-methoxy-1H-pyrrolo[2,3-c]pyridin-3-yl]-2-[4-(1-phenyltetrazol-5-yl)piperazin-1-yl]ethane-1,2-dione

HRID 1157773
ノート
印刷プレビュー

反応式

HRID 1157773 の反応式
Cl[C:2]1[N:3]=[CH:4][C:5]([O:32][CH3:33])=[C:6]2[C:10]([C:11](=[O:31])[C:12]([N:14]3[CH2:19][CH2:18][N:17]([C:20]4[N:24]([C:25]5[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=5)[N:23]=[N:22][N:21]=4)[CH2:16][CH2:15]3)=[O:13])=[CH:9][NH:8][C:7]=12.[O:34]1[CH2:38][CH2:37][O:36][CH:35]1[C:39]1[S:40][CH:41]=[C:42]([Sn](C)(C)C)[N:43]=1.N#N>O1CCOCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[O:34]1[CH2:38][CH2:37][O:36][CH:35]1[C:39]1[S:40][CH:41]=[C:42]([C:2]2[N:3]=[CH:4][C:5]([O:32][CH3:33])=[C:6]3[C:10]([C:11](=[O:31])[C:12]([N:14]4[CH2:19][CH2:18][N:17]([C:20]5[N:24]([C:25]6[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=6)[N:23]=[N:22][N:21]=5)[CH2:16][CH2:15]4)=[O:13])=[CH:9][NH:8][C:7]=23)[N:43]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 947NitrogenHCID 59511221HCID 59511221、化合物HCID 59511302HCID 59511302、化合物

生成物 1

HCID 497701741-[7-[2-(1,3-dioxolan-2-yl)thiazol-4-yl]-4-methoxy-1H-pyrrolo[2,3-c]pyridin-3-yl]-2-[4-(1-phenyltetrazol-5-yl)piperazin-1-yl]ethane-1,2-dione

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物
触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
100 °C

実験手順

To a sealable 75 mL flask containing 1-(7-chloro-4-methoxy-1H-pyrrolo[2,3-c]pyridin-3-yl)-2-(4-(1-phenyl-1H-tetrazol-5-yl)piperazin-1-yl)ethane-1,2-dione (0.3 g, 0.643 mmol) was added a solution of 2-(1,3-dioxolan-2-yl)-4-(trimethylstannyl)thiazole (0.210 g, 0.655 mmol) in 1,4-Dioxane (10 ml). The mixture was flushed with N2 and Pd(PPh3)4 (0.149 g, 0.129 mmol) was added. The mixture was again flushed with N2, and the flask was sealed and heated in an oil bath to 100° C. After 20 h of heating, the mixture was cooled to rt. The mixture was transferred to a rb flask using MeOH as the transfer solvent. The solvent was removed under reduced pressure. The residue was re-dissolved in DMF, and was passed through a pad of celite to remove any remaining solids. The DMF solution was purified by prep HPLC. After the prep HPLC, a mostly-pure sample was collected as an off-white solid. A small portion of this material was removed and re-purified by flash chromatography (0-5% MeOH in dichloromethane gradient) [20 mg after the purification]. The remainder of the product was carried forward to the next step with no additional purification (0.305 g). LCMS: m/e 588.1 (M+H)+, ret time 1.30 min (method 3). 1H NMR (500 MHz, DMSO-D6) δ ppm 12.20 (s, 1H) 8.38 (s, 1H) 8.22 (s, 1H) 8.11 (s, 1H) 7.68-7.72 (m, 2H) 7.57-7.66 (m, 3H) 6.29 (s, 1H) 4.16-4.20 (m, 2H) 4.07-4.10 (m, 2H) 3.99 (s, 3H) 3.67-3.71 (m, 2H) 3.41-3.45 (m, 2H) 3.30-3.32 (m, 2H) 3.15-3.19 (m, 2H).

後処理

  1. additionwas added
  2. customThe mixture was again flushed with N2
  3. customthe flask was sealed
  4. temperatureAfter 20 h of heating
  5. temperaturethe mixture was cooled to rt
  6. customThe mixture was transferred to a rb flask
  7. customThe solvent was removed under reduced pressure
  8. dissolutionThe residue was re-dissolved in DMF
  9. customto remove any remaining solids
  10. customThe DMF solution was purified by prep HPLC
  11. customAfter the prep HPLC, a mostly-pure sample was collected as an off-white solid
  12. customA small portion of this material was removed
  13. customre-purified by flash chromatography (0-5% MeOH in dichloromethane gradient) [20 mg
  14. customafter the purification]
  15. customThe remainder of the product was carried forward to the next step with no additional purification (0.305 g)
  16. customm/e 588.1 (M+H)+, ret time 1.30 min (method 3)

出典と根拠

ORDレコード
ord-5f87bdca158f442f930cee1f0224d941
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07807676B2

反応ノート

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