4-[N-Dodecyl-N-[2-[4-(3,3-Dimethoxy-4,4,4-trifluorobut-1-yl)phenoxy]ethyl]amino]butanoic acid, ethyl ester → 4-[N-dodecyl-N-[2-[4-(3oxo-4,4,4-trifluorobut-1-yl)phenoxy]ethyl]amino]butanoic acid, ethyl ester

HRID 1383932노트

반응식

HRID 1383932 반응식
[CH2:1]([N:13]([CH2:34][CH2:35][CH2:36][C:37]([O:39][CH2:40][CH3:41])=[O:38])[CH2:14][CH2:15][O:16][C:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH2:24][C:25](OC)([O:30]C)[C:26]([F:29])([F:28])[F:27])=[CH:19][CH:18]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]>FC(F)(F)C(O)=O>[CH2:1]([N:13]([CH2:34][CH2:35][CH2:36][C:37]([O:39][CH2:40][CH3:41])=[O:38])[CH2:14][CH2:15][O:16][C:17]1[CH:18]=[CH:19][C:20]([CH2:23][CH2:24][C:25](=[O:30])[C:26]([F:27])([F:28])[F:29])=[CH:21][CH:22]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]

참가 물질

3

반응물 1

HCID 867571324-[N-Dodecyl-N-[2-[4-(3,3-Dimethoxy-4,4,4-trifluorobut-1-yl)phenoxy]ethyl]amino]butanoic acid, ethyl ester

생성물 1

HCID 867571224-[N-dodecyl-N-[2-[4-(3oxo-4,4,4-trifluorobut-1-yl)phenoxy]ethyl]amino]butanoic acid, ethyl ester수율 77.7%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of 4[N-Dodecyl-N-[2-[4-(3,3-dimethoxy-4,4,4-trifluorobut-1-yl)phenoxy]ethyl]amino]-butanoic acid, ethyl ester (315 mg, 0.53 mmol) in trifluoroacetic acid (5 ml) was heated to 70° C. for 2 h, and then concentrated in vacuo. The residue was diluted with ethyl acetate (100 ml), washed with sat. sodium bicarbonate (30 ml), brine (30 ml), dried over magnesium sulfate and concentrated in vacuo. The residue was chromatographed on silica gel (Hexane/ethyl acetate 2:1 to 1.5:1) to afford the title compound (224 mg, 77%) as a colorless oil.

후처리

  1. concentrationconcentrated in vacuo
  2. additionThe residue was diluted with ethyl acetate (100 ml)
  3. washwashed with sat. sodium bicarbonate (30 ml), brine (30 ml)
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe residue was chromatographed on silica gel (Hexane/ethyl acetate 2:1 to 1.5:1)

출처 및 근거

ORD 기록
ord-95ca9d0b89dc47ae81ba5299093c4641
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06255496B1

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