4-Bromophenol → HCID 59589836、化合物

HRID 1054374ノート

反応式

HRID 1054374 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.[CH3:9][N:10]([CH3:15])[CH2:11][C@@H:12](O)[CH3:13].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OC(C)(C)C)=O)=NC(OC(C)(C)C)=O>ClCCl>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][C@H:12]([CH3:13])[CH2:11][N:10]([CH3:15])[CH3:9])=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 78084-BromophenolHCID 11776TriphenylphosphineHCID 97268Di-tert-butyl azodicarboxylateHCID 6950248(S)-(+)-1-Dimethylamino-2-propanol

生成物 1

HCID 59589836HCID 59589836、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

4-Bromophenol (0.2 g, 1.16 mmol) and (S)-(+)-1-dimethylamino-2-propanol (0.14 ml, 1.16 mmol) were dissolved in dichloromethane (10 ml). PS-Triphenylphospine (1.74 g, 1.74 mmol) was added, followed by di-tert-butyl azodicarboxylate (0.4 g, 1.74 mmol). The mixture was stirred overnight at room temperature, then filtered and the filtrate washed with sodium hydrogenocarbonate then brine. The organic phase was dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to give the desired product. Yield: 0.3 g, 100%. LCMS method: 2, RT: 2.62 min; MI: 258-260 [M+1].

後処理

  1. filtrationfiltered
  2. washthe filtrate washed with sodium hydrogenocarbonate
  3. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-ab732a84b1b649bfb5c381606c87d682
出典データセット
uspto-grants-2016_07
特許番号
US09394301B2

反応ノート

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