Trifluoroacetic acid → HCID 66714093, 화합물

HRID 2173764노트

반응식

HRID 2173764 반응식
[N:1]1([CH2:7][CH2:8][O:9][CH2:10][CH2:11][O:12][CH2:13][CH2:14][O:15][CH2:16][CH2:17][C:18]([O:20]C(C)(C)C)=[O:19])[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[N:1]1([CH2:7][CH2:8][O:9][CH2:10][CH2:11][O:12][CH2:13][CH2:14][O:15][CH2:16][CH2:17][C:18]([OH:20])=[O:19])[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 66716176HCID 66716176, 화합물

생성물 1

HCID 66714093HCID 66714093, 화합물수율 99%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 1 g of tert-butyl 3-{2-[2-(2-morpholin-4-yl-ethoxy)-ethoxy]-ethoxy}-propanoate in 50 ml of DCM was added 4 ml of TFA. The mixture was stirred for 10 hours at room temperature and then concentrated under reduced pressure and purified on a Mega BE-SCX, 25GM 150ML cartridge (Varian), using washing with MeOH and detachment of the expected product with a 2N solution of ammonia in MeOH. The fractions containing the desired product were combined and concentrated under reduced pressure. 830 mg of 3-{2-[2-(2-morpholin-4-yl-ethoxy)-ethoxy]-ethoxy}-propanoic acid were obtained. LC/MS (E): tr (ELSD)=0.16 min; [M+H]+: m/z 292

후처리

  1. concentrationconcentrated under reduced pressure
  2. custompurified on a Mega BE-SCX, 25GM 150ML cartridge (Varian)
  3. washusing washing with MeOH and detachment of the expected product with a 2N solution of ammonia in MeOH
  4. additionThe fractions containing the desired product
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-34f9624ce5e64cbbb4ef9bb13ec151a5
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09056914B2

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