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5-Bromopyrimidine → HCID 16069044, 화합물

HRID 2047569
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HRID 2047569 반응식
[N:1]1([C@@H:7]2[CH2:10][C@H:9]([C:11]3[S:12][C:13]4[CH:19]=[C:18]([NH2:20])[CH:17]=[CH:16][C:14]=4[N:15]=3)[CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Br[C:22]1[CH:23]=[N:24][CH:25]=[N:26][CH:27]=1.C1(P(C2C=CC=CC=2)C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(C)([O-])C.[Na+]>O.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(C)C=CC=CC=1>[N:1]1([CH:7]2[CH2:10][CH:9]([C:11]3[S:12][C:13]4[CH:19]=[C:18]([NH:20][C:22]5[CH:23]=[N:24][CH:25]=[N:26][CH:27]=5)[CH:17]=[CH:16][C:14]=4[N:15]=3)[CH2:8]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 783445-BromopyrimidineHCID 634876Binap, (A+-)-HCID 23676156Sodium t-butoxideHCID 178507336HCID 178507336, 화합물

생성물 1

HCID 16069044HCID 16069044, 화합물

시약·촉매·용매 3

HCID 9811564Bis(dibenzylideneacetone)palladium
촉매
HCID 962Water용매
HCID 1140Toluene용매

반응 조건

온도
145 °C

실험 절차

The product of Example 101A (cis-2-(3-piperidin-1-yl-cyclobutyl)-benzothiazole-6-ylamine) (50 mg, 0.174 mmole), 5-bromopyrimidine (42 mg, 0.264 mmole), tris(dibenzylideneacetone)dipalladium (0) (6.5 mg, 0.007 mmole), racemic-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (BINAP, 8.7 mg, 0.014 mmole) and sodium tert-butoxide (23 mg, 0.242 mmole) were charged in a tube and sealed. The tube was placed on high vacuum for 2 hours and refilled with nitrogen. Toluene (2 mL) was added and the reaction vessel was placed in a microwave reactor and heated at 145° C. for 15 minutes. After cooling to room temperature, the mixture was diluted with water and extracted three times with dichloromethane. The combined organic layers were concentrated and the crude product was purified by column chromatography (0.4% ammonium hydroxide and 4% methanol in dichloromethane). The product collected was a mixture of cis and trans isomers. 1H NMR (400 MHz, CDCl3) δ ppm 8.79 (s, 1H) 8.50-8.56 (m, 2H) 7.89 (d, J=8.90 Hz, 1H) 7.58 (d, J=2.15 Hz, 1H) 7.18 (dd, J=8.59, 2.15 Hz, 1H) 5.83 (s, 1H) 3.48-3.63 (m, 1H) 2.73-2.85 (m, 1H) 2.59-2.71 (m, 2H) 2.23-2.39 (m, 6H) 1.54-1.66 (m, 4H) 1.41-1.51 (m, 2H). MS: (M+H)+=366.

후처리

  1. customsealed
  2. additionrefilled with nitrogen
  3. customthe reaction vessel was placed in a microwave reactor
  4. temperatureAfter cooling to room temperature
  5. extractionextracted three times with dichloromethane
  6. concentrationThe combined organic layers were concentrated
  7. customthe crude product was purified by column chromatography (0.4% ammonium hydroxide and 4% methanol in dichloromethane)
  8. customThe product collected
  9. additiona mixture of cis and trans isomers

출처 및 근거

ORD 기록
ord-585622fd7f2b40a097960c915a0eeac0
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08592467B2

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