Triphenylphosphine → HCID 67298266、化合物

HRID 1520397ノート

反応式

HRID 1520397 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 67298266HCID 67298266、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
50 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-17fb77be2ebd484e878d4d688d24980e
出典データセット
uspto-grants-2015_07
特許番号
US09073890B2

反応ノート

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