Hydrochloric Acid → HCID 59416079, 화합물

HRID 2061812노트

반응식

HRID 2061812 반응식
[CH2:1]([NH:3][C:4](=[O:45])[NH:5][C:6]1[N:11]=[CH:10][C:9]([C:12]2[CH:13]=[C:14]3[C:19](=[CH:20][CH:21]=2)[N:18]([C:22]2([CH2:28][OH:29])[CH2:27][CH2:26][O:25][CH2:24][CH2:23]2)[CH:17]=[C:16]([C:30]([O:32]CC)=[O:31])[C:15]3=[O:35])=[C:8]([C:36]2[S:37][CH:38]=[C:39]([C:41]([F:44])([F:43])[F:42])[N:40]=2)[CH:7]=1)[CH3:2].C1COCC1.[Li+].[OH-].Cl>CO>[CH2:1]([NH:3][C:4](=[O:45])[NH:5][C:6]1[N:11]=[CH:10][C:9]([C:12]2[CH:13]=[C:14]3[C:19](=[CH:20][CH:21]=2)[N:18]([C:22]2([CH2:28][OH:29])[CH2:27][CH2:26][O:25][CH2:24][CH2:23]2)[CH:17]=[C:16]([C:30]([OH:32])=[O:31])[C:15]3=[O:35])=[C:8]([C:36]2[S:37][CH:38]=[C:39]([C:41]([F:44])([F:42])[F:43])[N:40]=2)[CH:7]=1)[CH3:2]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 44540255HCID 44540255, 화합물

생성물 1

HCID 59416079HCID 59416079, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
100 °C

실험 절차

Ethyl 6-(6-(3-ethylureido)-4-(4-(trifluoromethyl)thiazol-2-yl)pyridin-3-yl)-1-(4-(hydroxymethyl)tetrahydro-2H-pyran-4-yl)-4-oxo-1,4-dihydroquinoline-3-carboxylate (Example 132, 0.225 g, 0.35 mmol) was diluted with 2:1 MeOH:THF (3 mL). A 2 M aq solution of LiOH (0.35 mL, 0.7 mmol) was added and the reaction mixture was heated in the microwave to 100° C. for 15 min. The mixture was conc in vacuo and acidified to approx. pH 3 with 1 N aq HCl. The resultant solid was collected and purified by column chromatography (silica 95:5 methylene chloride/methanol) followed by purification by reverse phase HPLC (C18, 0-95% acetonitrile/water gradient).

후처리

  1. customThe resultant solid was collected
  2. custompurified by column chromatography (silica 95:5 methylene chloride/methanol)
  3. customfollowed by purification by reverse phase HPLC (C18, 0-95% acetonitrile/water gradient)

출처 및 근거

ORD 기록
ord-68610ee6058745b8bb0bf305a99e52b5
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08283361B2

반응 노트

불러오는 중…