Triphenylphosphine → HCID 67298266, 화합물

HRID 1520397노트

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HRID 1520397 반응식
[OH:1][CH2:2][C:3]1[CH:13]=[CH:12][C:6]2[N:7]([CH3:11])[C:8](=[O:10])[O:9][C:5]=2[CH:4]=1.[CH3:14][NH:15][C:16]1[C:25]2[C:20](=[CH:21][CH:22]=[C:23]([C:26]3[CH:27]=[C:28](O)[CH:29]=[CH:30][CH:31]=3)[CH:24]=2)[N:19]=[C:18]([C:33]2[CH:34]=[N:35][CH:36]=[CH:37][CH:38]=2)[N:17]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1C=CC(COC(/N=N/C(OCC2C=CC=CC=2)=O)=O)=CC=1>C1COCC1>[CH3:11][N:7]1[C:6]2[CH:12]=[CH:13][C:3]([CH2:2][O:1][C:30]3[CH:29]=[CH:28][CH:27]=[C:26]([C:23]4[CH:24]=[C:25]5[C:20](=[CH:21][CH:22]=4)[N:19]=[C:18]([C:33]4[CH:34]=[N:35][CH:36]=[CH:37][CH:38]=4)[N:17]=[C:16]5[NH:15][CH3:14])[CH:31]=3)=[CH:4][C:5]=2[O:9][C:8]1=[O:10]

참가 물질

6

반응물 4

HCID 11776TriphenylphosphineHCID 5387121Dibenzyl azodicarboxylateHCID 541295736-(hydroxymethyl)-3-methyl-2,3-dihydro-1,3-benzoxazol-2-oneHCID 67297993HCID 67297993, 화합물

생성물 1

HCID 67298266HCID 67298266, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
50 °C

실험 절차

To 6-(hydroxymethyl)-3-methylbenzo[d]oxazol-2(3H)-one (45.1 μmol) was added the solution of 3-(4-(methylamino)-2-(pyridin-3-yl)quinazolin-6-yl)phenol (30 μmol) in THF (400 μL). After PS-triphenylphosphine (60 μmol) was added, the solution of DBAD (di-tert-butyl azodicarboxylate, 66 mmol) in THF was dispensed to the vials. The mixture was heated at 50° C. for 8 h. After the solvent was removed, the residue was diluted with methanol and purified by Mass triggered PREP-HPLC Condition D. The target fraction was lyophilized to afford the titled compound whose structure was finally confirmed by LCMS using LCMS Method E.

후처리

  1. customAfter the solvent was removed
  2. additionthe residue was diluted with methanol
  3. custompurified by Mass

출처 및 근거

ORD 기록
ord-17fb77be2ebd484e878d4d688d24980e
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073890B2

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