4-Bromophenol → HCID 59589836, 화합물

HRID 1054374노트

반응식

HRID 1054374 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 59589836HCID 59589836, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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].

후처리

  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

출처 및 근거

ORD 기록
ord-ab732a84b1b649bfb5c381606c87d682
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394301B2

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