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Triphenylphosphine → HCID 18767693, 화합물

HRID 2105677
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HRID 2105677 반응식
[C:1]([CH2:3][CH2:4][NH:5][C:6](=O)[CH2:7][CH2:8][C:9]12[CH2:16][CH2:15][C:12]([C:17]3[NH:25][C:24]4[C:23](=[O:26])[N:22]([CH2:27][CH2:28][CH3:29])[C:21](=[O:30])[N:20]([CH2:31][CH2:32][CH3:33])[C:19]=4[N:18]=3)([CH2:13][CH2:14]1)[CH2:11][CH2:10]2)#[N:2].C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.[Si]([N:58]=[N+:59]=[N-:60])(C)(C)C.CCOC(/N=N/C(OCC)=O)=O>C1COCC1>[O:30]=[C:21]1[N:20]([CH2:31][CH2:32][CH3:33])[C:19]2[N:18]=[C:17]([C:12]34[CH2:15][CH2:16][C:9]([CH2:8][CH2:7][C:6]5[N:5]([CH2:4][CH2:3][C:1]#[N:2])[N:60]=[N:59][N:58]=5)([CH2:14][CH2:13]3)[CH2:10][CH2:11]4)[NH:25][C:24]=2[C:23](=[O:26])[N:22]1[CH2:27][CH2:28][CH3:29]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 78378AzidotrimethylsilaneHCID 5462977Diethyl azodicarboxylateHCID 18767616HCID 18767616, 화합물

생성물 1

HCID 18767693HCID 18767693, 화합물수율 3.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

A solution of N-(2-cyano-ethyl)-3-[4-(2,6-dioxo-1,3-dipropyl-2,3,6,7-tetrahydro-1H-purin-8-yl)-bicyclo[2.2.2]oct-1-yl]-propionamide (500 ng, 1.06 mmol, 1.0 eq), Ph3P (2.0 eq, 2.13 mmol, 560 mg), TMSN3 (2.0 eq, 2.13 mmol, 245 mg), and DEAD (2.0 eq, 2.13 mmol, 371 mg) in THF (10 ml) was stirred at rt for 24 h. The reaction vessel was re-charged with the reagent cocktail (2.0 eq, 2.13 mmol) and stirring was continued for an additional 24 h. The reaction was quenched by the addition of a 50% aqueous solution of (NH4)2Ce(NO3)6 and extracted with EtOAc. The combined organic extracts were washed with brine, dried over MgSO4, filtered and evaporated in vacuo to afford a viscous orange oil. A portion of the material was purified by preparative LC to afford 20 mg of pure material. MS: 494 (MH+).

후처리

  1. additionThe reaction vessel was re-charged with the reagent cocktail (2.0 eq, 2.13 mmol)
  2. customThe reaction was quenched by the addition of a 50% aqueous solution of (NH4)2Ce(NO3)6
  3. extractionextracted with EtOAc
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. customevaporated in vacuo
  8. customto afford a viscous orange oil
  9. customA portion of the material was purified by preparative LC

출처 및 근거

ORD 기록
ord-475d56c461c64571b6f0c58f8e6972b8
출처 데이터셋
uspto-grants-2009_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07579354B2

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