Diphenylphosphine → HCID 90415270、化合物

HRID 57383

反応式

HRID 57383 の反応式
C1(PC2C=CC=CC=2)C=CC=CC=1.[N:14]([CH:17]([C:19]1[O:20][C:21]([C:25]2[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=2)=[C:22]([CH3:24])[N:23]=1)[CH3:18])=[N+]=[N-]>CO>[Cl:31][C:28]1[CH:27]=[CH:26][C:25]([C:21]2[O:20][C:19]([CH:17]([NH2:14])[CH3:18])=[N:23][C:22]=2[CH3:24])=[CH:30][CH:29]=1

参加物

4

反応物 2

HCID 70017DiphenylphosphineHCID 904151212-(1-Azidoethyl)-5-(4-chlorophenyl)-4-methyloxazole

生成物 1

HCID 90415270HCID 90415270、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

SiliaBond® Diphenylphosphine (1500 mg, 1.19 mmol/g) was added to a solution of 2-(1-azidoethyl)-5-(4-chlorophenyl)-4-methyloxazole (366 mg, 1.393 mmol) in anhydrous methanol (15 ml) and shaken for 3 hours. The reaction was filtered and concentrated in vacuo. Flash column chromatography (silica, 40 g) eluting with 2-10% MeOH/DCM afforded 160 mg (white solid). HRMS(B) tR=1.73 min; MS m/z 236.0716

後処理

  1. filtrationThe reaction was filtered
  2. concentrationconcentrated in vacuo
  3. washFlash column chromatography (silica, 40 g) eluting with 2-10% MeOH/DCM
  4. customafforded 160 mg (white solid)

出典と根拠

ORDレコード
ord-03856303fa484d6eb768a8b464c01e01
出典データセット
uspto-grants-2016_09
特許番号
US09434719B2

関連ノート

読み込み中…