Hydrochloric Acid → 2-[(3-{4-[(benzyl{2-methyl-3-[(methylsulfonyl)amino]phenyl}amino)methyl]phenoxy}phenoxy)methyl]cyclopropanecarboxylic Acid

HRID 1370963노트

반응식

HRID 1370963 반응식
[CH2:1]([N:8]([CH2:21][C:22]1[CH:44]=[CH:43][C:25]([O:26][C:27]2[CH:28]=[C:29]([CH:40]=[CH:41][CH:42]=2)[O:30][CH2:31][CH:32]2[CH2:34][CH:33]2[C:35]([O:37]CC)=[O:36])=[CH:24][CH:23]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([NH:15][S:16]([CH3:19])(=[O:18])=[O:17])[C:10]=1[CH3:20])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.O1CCCC1>O>[CH2:1]([N:8]([CH2:21][C:22]1[CH:23]=[CH:24][C:25]([O:26][C:27]2[CH:28]=[C:29]([CH:40]=[CH:41][CH:42]=2)[O:30][CH2:31][CH:32]2[CH2:34][CH:33]2[C:35]([OH:37])=[O:36])=[CH:43][CH:44]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([NH:15][S:16]([CH3:19])(=[O:18])=[O:17])[C:10]=1[CH3:20])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 18511920Ethyl 2-((3-(4-((benzyl(2-methyl-3-((methylsulfonyl)amino)phenyl)amino)methyl)phenoxy)phenoxy)methyl)cyclopropanecarboxylate

생성물 1

HCID 101211712-[(3-{4-[(benzyl{2-methyl-3-[(methylsulfonyl)amino]phenyl}amino)methyl]phenoxy}phenoxy)methyl]cyclopropanecarboxylic Acid

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

To the product from Example 284A was added 2N hydrochloric acid (1 mL), tetrahydrofuran (0.5 mL) and water (0.5 mL). The reaction mixture was stirred at room temperature overnight. Water (2 mL) was added. The solution was neutralized with 1N hydrochloric aid until pH=2˜3. The product was extracted with ethyl acetate (2 mL), dried in vaccuo, and purified by HPLC to provide the titled compound. 1H NMR (500 MHz, DMSO-d6) δ12.01-12.29 (br.s, 1 H), 8.95 (s, 1 H), 7.23 (m, 8 H), 7.03 (m, 1 H), 6.94 (m, 4 H), 6.69 (m, 1 H), 6.50 (m, 2 H), 4.06 (s, 2 H), 4.03 (s, 2 H), 3.94 (m, 1 H), 3.80 (m, 1 H), 2.91 (s, 3 H), 2.40 (s, 3 H), 1.67 (m, 1 H), 1.57 (m, 1 H), 1.05 (m, 1 H), 0.92 (m, 1 H); MS (APCI+) m/z 587.1 (M+H)+.

후처리

  1. extractionThe product was extracted with ethyl acetate (2 mL)
  2. customdried in vaccuo
  3. custompurified by HPLC

출처 및 근거

ORD 기록
ord-0160176a53eb4974abc93d73f80a24c4
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06583180B2

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