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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Triphenylphosphine → HCID 57764525, 화합물

HRID 402319
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HRID 402319 반응식
[NH2:1][C:2]1[C:3]2[N:10]=[C:9](Br)[N:8]([C@@H:12]3[O:18][C@H:17]([CH2:19][OH:20])[C@@H:15]([OH:16])[C@H:13]3[OH:14])[C:4]=2[N:5]=[N:6][N:7]=1.[CH:21]1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C[Al](C)C>C[Si](C)(C)N[Si](C)(C)C.C1COCC1.Cl[Pd]Cl>[NH2:1][C:2]1[C:3]2[N:10]=[C:9]([CH3:21])[N:8]([C@@H:12]3[O:18][C@H:17]([CH2:19][OH:20])[C@@H:15]([OH:16])[C@H:13]3[OH:14])[C:4]=2[N:5]=[N:6][N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 11776TriphenylphosphineHCID 16682925TrimethylaluminumHCID 57764505HCID 57764505, 화합물

생성물 1

HCID 57764525HCID 57764525, 화합물수율 310%

시약·촉매·용매 3

HCID 24290Palladium Chloride촉매HCID 8028Tetrahydrofuran
용매
HCID 13838Hexamethyldisilazane용매

실험 절차

The compound from Step A (112 mg, 0.3 mmol) was heated at reflux in hexamethyldisilazane (15 mL) for 16 hours. The mixture was evaporated to dryness to give a syrup which was dissolved in dry THF (12 mL). PPh3 (10 mg; 0.04 mmol), PdCl2 (3.5 mg; 0.02 mmol) and AlMe3 (100 μl; 0.94 mmol) were added. The mixture was reflux for 5 hours. The mixture was evaporated to dryness. The crude product was dissolved in methanol (30 mL) in the presence of ammonium chloride. The mixture was evaporated to dryness and the residue was purified on silica gel reverse-phase (C18) using water/acetonitrile (from 9/1 to 6/4) as eluant to give the title compound (35 mg) as a yellow powder.

후처리

  1. customThe mixture was evaporated to dryness
  2. customto give a syrup which
  3. temperatureThe mixture was reflux for 5 hours
  4. customThe mixture was evaporated to dryness
  5. dissolutionThe crude product was dissolved in methanol (30 mL) in the presence of ammonium chloride
  6. customThe mixture was evaporated to dryness
  7. customthe residue was purified on silica gel reverse-phase (C18)

출처 및 근거

ORD 기록
ord-8d8c12bca64c40d9bbeecfa2099f6493
출처 데이터셋
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08742101B2

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