Epibromohydrin → HCID 86729263, 화합물

HRID 1051483노트

반응식

HRID 1051483 반응식
[OH:1][C:2]1[CH:3]=[C:4]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH:5]=[CH:6][CH:7]=1.[H-].[Na+].Br[CH2:19][CH:20]1[CH2:22][O:21]1>CN(C=O)C>[O:21]1[CH2:22][CH:20]1[CH2:19][O:1][C:2]1[CH:3]=[C:4]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:12])([CH3:14])[CH3:13])[CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 18430EpibromohydrinHCID 24758Sodium hydrideHCID 312485tert-butyl N-(3-hydroxyphenyl)carbamate

생성물 1

HCID 86729263HCID 86729263, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of tert-butyl (3-hydroxyphenyl)carbamate (1 g, 4.79 mmol) in DMF (15 mL) was added NaH (0.126 g, 5.26 mmol) at 0° C. After stirring for 30 min, 2-(bromomethyl)oxirane (0.716 g, 5.26 mmol) was added and the mixture stirred at 0° C. for 1 h before quenching with the addition of MeOH. After evaporation of this mixture, the resulting residue was dissolved in ethyl acetate and washed with water, dried and with sodium sulfate and concentrated with the resulting crude product used for next step without further purification.

후처리

  1. stirringthe mixture stirred at 0° C. for 1 h
  2. custombefore quenching with the addition of MeOH
  3. customAfter evaporation of this mixture
  4. dissolutionthe resulting residue was dissolved in ethyl acetate
  5. washwashed with water
  6. dry with materialdried and with sodium sulfate
  7. concentrationconcentrated with the resulting crude product
  8. customused for next step without further purification

출처 및 근거

ORD 기록
ord-c350ac3bce2f48b18ea222fe6cb96c08
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09388173B2

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