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Water → Tert-butyl 3-(3-chloro-5-(1-chloroethyl)-2-fluoro-6-methoxyphenyl)azetidine-1-carboxylate

HRID 510946
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HRID 510946 반응식
N1C(Cl)=NC(Cl)=NC=1[Cl:3].CN(C=O)C.[Cl:15][C:16]1[C:17]([F:38])=[C:18]([CH:27]2[CH2:30][N:29]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:28]2)[C:19]([O:25][CH3:26])=[C:20]([CH:22](O)[CH3:23])[CH:21]=1.O>ClCCl>[Cl:15][C:16]1[C:17]([F:38])=[C:18]([CH:27]2[CH2:30][N:29]([C:31]([O:33][C:34]([CH3:37])([CH3:36])[CH3:35])=[O:32])[CH2:28]2)[C:19]([O:25][CH3:26])=[C:20]([CH:22]([Cl:3])[CH3:23])[CH:21]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 6228DimethylformamideHCID 7954Cyanuric chlorideHCID 86666860Tert-butyl 3-(3-chloro-2-fluoro-5-(1-hydroxyethyl)-6-methoxyphenyl)azetidine-1-carboxylate

생성물 1

HCID 86666861Tert-butyl 3-(3-chloro-5-(1-chloroethyl)-2-fluoro-6-methoxyphenyl)azetidine-1-carboxylate수율 53.2%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매
2회

실험 절차

Cyanuric chloride (140 mg, 0.78 mmol) was added to DMF (0.059 mL, 0.77 mmol) at room temperature. After the formation of a white solid (10 min), methylene chloride (4 mL) was added, followed by tert-butyl 3-[3-chloro-2-fluoro-5-(1-hydroxyethyl)-6-methoxyphenyl]azetidine-1-carboxylate (197 mg, 0.547 mmol). After the addition, the mixture was stirred at room temperature overnight. Water was added, and the resulting mixture was then diluted with dichloromethane. The organic phase was separated, washed with sat. NaHCO3 solution, water and brine, dried over MgSO4, concentrated and purified on silica gel (eluting with 0 to 30% EtOAc in hexanes) to give the desired product (110 mg, 53%).

후처리

  1. additionAfter the addition
  2. customThe organic phase was separated
  3. washwashed with sat. NaHCO3 solution, water and brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. custompurified on silica gel (eluting with 0 to 30% EtOAc in hexanes)

출처 및 근거

ORD 기록
ord-0bd0d5a79a07465ca82d1b43eeaf90c4
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09096600B2

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