Water → Ethyl morpholinoethyl 3-trifluoromethylbenzylphosphonate

HRID 1733822노트

반응식

HRID 1733822 반응식
[CH2:1]([O:3][P:4]([CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:9]=1)(Cl)=[O:5])[CH3:2].[OH:18][CH2:19][CH2:20][N:21]1[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1.C(N(CC)CC)C.O>C(Cl)Cl>[F:17][C:14]([F:15])([F:16])[C:10]1[CH:9]=[C:8]([CH:13]=[CH:12][CH:11]=1)[CH2:7][P:4](=[O:5])([O:18][CH2:19][CH2:20][N:21]1[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1)[O:3][CH2:1][CH3:2]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 611632-MorpholinoethanolHCID 158191953-Trifluoromethylbenzylphosphonochloridic acid ethyl ester

생성물 1

HCID 15818099Ethyl morpholinoethyl 3-trifluoromethylbenzylphosphonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

3-Trifluoromethylbenzylphosphonochloridic acid ethyl ester (7.0 mmol)in 20 mL of CH2Cl2 is added slowly to a mixture of N-(2-hydroxyethyl)morpholine and triethylamine (7 mmol) in 20 mL of CH2Cl2 cooled in an ice bath. The resultant mixture is allowed to reach room temperature and is stirred for 5 hours. Water is added (100 mL) and the aqueous phase is extracted 3 times with CH2Cl2 (3×100 mL). The combined organic extracts are dried with anhydrous MgSO4, and evaporated to give the desired product.

후처리

  1. temperaturecooled in an ice bath
  2. customto reach room temperature
  3. extractionthe aqueous phase is extracted 3 times with CH2Cl2 (3×100 mL)
  4. dry with materialThe combined organic extracts are dried with anhydrous MgSO4
  5. customevaporated

출처 및 근거

ORD 기록
ord-b9a01b15cf394c678d84216bc5754ffa
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05532226

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