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HCID 66614869, 화합물 → HCID 58571264, 화합물

HRID 717623
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HRID 717623 반응식
CC1(C)[O:7][CH2:6][C:5]([C:9]#[C:10][C:11]2[CH:16]=[CH:15][C:14]([CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:13][CH:12]=2)([OH:8])[CH2:4][O:3]1>C(O)(C(F)(F)F)=O.CCO.[Pd]>[CH2:17]([C:14]1[CH:15]=[CH:16][C:11]([CH2:10][CH2:9][C:5]([OH:8])([CH2:6][OH:7])[CH2:4][OH:3])=[CH:12][CH:13]=1)[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 1

HCID 66614869HCID 66614869, 화합물

생성물 1

HCID 58571264HCID 58571264, 화합물수율 100.6%

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 702Ethanol용매HCID 6422Trifluoroacetic acid용매

실험 절차

A mixture of the product of Step B (0.03 g; 0.087 mmol) and 10% Pd/C (0.05 g) in 5% TFA in EtOH (10 ml) was stirred for 1 h under H2 (balloon) at room temperature, then filtered through a pad of Celite, washed with CH2Cl2 (2×10 ml). To combined filtrates were evaporated to dryness under reduced pressure and dried in vacuo for 1 h to give title compound (0.027 g; 99%) as a colourless solid. 1H-NMR (CDCl3) 7.05 (s, 4H); 3.66 (broad m, 7H); 2.61 (m, 2H); 2.51 (t, 2H, J=7.92 Hz); 1.73 (m 2H); 1.55 (t, 3H, J=6.93 Hz); 1.26 (m, 10H); 0.87 (t, 3H, J=6.93 Hz).

후처리

  1. filtrationfiltered through a pad of Celite
  2. washwashed with CH2Cl2 (2×10 ml)
  3. customwere evaporated to dryness under reduced pressure
  4. customdried in vacuo for 1 h

출처 및 근거

ORD 기록
ord-ece6ecadc8fc4ba5b5c4997841096b8e
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09193716B2

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