Sodium Hydroxide → HCID 53921056, 화합물

HRID 1281448노트

반응식

HRID 1281448 반응식
[Br:1][C:2]1[CH:3]=[C:4]([C:31]([NH:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][C:42]2C=C[CH:45]=[CH:44][CH:43]=2)=[O:32])[CH:5]=[C:6]([C:21]2[CH:26]=[CH:25][CH:24]=[C:23]([C:27]([F:30])([F:29])[F:28])[CH:22]=2)[C:7]=1[O:8][CH2:9][CH2:10][NH:11][C:12]([NH:14]C(=O)C(Cl)(Cl)Cl)=[O:13].[OH-].[Na+]>C(Cl)Cl.CO>[CH2:34]([NH:33][C:31]([C:4]1[CH:5]=[C:6]([C:21]2[CH:26]=[CH:25][CH:24]=[C:23]([C:27]([F:30])([F:28])[F:29])[CH:22]=2)[C:7]([O:8][CH2:9][CH2:10][NH:11][C:12]([NH2:14])=[O:13])=[C:2]([Br:1])[CH:3]=1)=[O:32])[CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH3:45]

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 22237643HCID 22237643, 화합물

생성물 1

HCID 53921056HCID 53921056, 화합물수율 92%

시약·촉매·용매 1

HCID 21226129Dichloromethane methanol용매

실험 절차

To a solution of 5-bromo-N-(8-phenyloctyl)-6-[2-({[(2,2,2-trichloroacetyl)amino]carbonyl}amino)ethoxy]-3′-(trifluoromethyl)[1,1′-biphenyl]-3-carboxamide in CH2Cl2/MeOH (10/4) (14 mL) was added 1M NaOH (2 mL). The reaction was stirred at rt overnight and concentrated in vacuo. The residue was extracted with CH2Cl2, dried over MgSO4 and concentrated in vacuo. The residue was purified by flash chromatography (3 to 5% MeOH:CH2Cl2) to afford the title compound (0.203 g, 92%) as a white solid. mp 122.5-125.1° C. 1H NMR (DMSO-d6) δ 8.58 (bt, 1H); 8.12 (d, 1H); 7.90 (m, 3H); 7.78 (d, 1H); 7.73 (dd, 1H); 6.95 (t, 1H); 5.44 (s, 2H); 3.48 (dd, 2H); 3.24 (dd, 2H); 3.05 (ddd, 2H); 1.48 (dd, 2H); 1.25 (m, 18H); 0.84 (t, 3H); (KBr) 3300, 2950, 2820, 1650, 1600, 1550, 1460, 1330, 1180, 1120, 1080, 1030, 900, 805 cm−1; mass spectrum [(+)ESI], m/z 614/616 (M+H)+; Anal. Calcd. for C29H39BrF3N3O3: C, 56.68; H, 6.40; N, 6.84, Found: C, 56.37; H, 6.25; N, 6.49.

후처리

  1. concentrationconcentrated in vacuo
  2. extractionThe residue was extracted with CH2Cl2
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash chromatography (3 to 5% MeOH:CH2Cl2)

출처 및 근거

ORD 기록
ord-81995bead19f45dea45520d3c29d7ff5
출처 데이터셋
uspto-grants-2002_09
특허 번호
US06451827B2

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