홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Lithium Hydroxide → HCID 22730282, 화합물

HRID 2356134
노트
인쇄 미리보기

반응식

HRID 2356134 반응식
CO[C:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH2:12][CH2:13][N:14]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:15][CH:16]=2)=[CH:7][CH:6]=1)=[O:4].[Li+].[OH-].[N+:26]([C:29]1[CH:30]=[C:31]([S:45]([NH2:48])(=[O:47])=[O:46])[CH:32]=[CH:33][C:34]=1[NH:35][CH2:36][CH2:37][S:38][C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1)([O-:28])=[O:27].CCN=C=NCCCN(C)C>C1COCC1.CO.CN(C1C=CN=CC=1)C.ClC(Cl)C.C(OCC)(=O)C.O>[N+:26]([C:29]1[CH:30]=[C:31]([S:45]([NH:48][C:3]([C:5]2[CH:10]=[CH:9][C:8]([C:11]3[CH2:12][CH2:13][N:14]([C:17]([O:19][C:20]([CH3:23])([CH3:22])[CH3:21])=[O:18])[CH2:15][CH:16]=3)=[CH:7][CH:6]=2)=[O:4])(=[O:46])=[O:47])[CH:32]=[CH:33][C:34]=1[NH:35][CH2:36][CH2:37][S:38][C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1)([O-:28])=[O:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 4

HCID 3939Lithium HydroxideHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 8461424HCID 8461424, 화합물HCID 22730763HCID 22730763, 화합물

생성물 1

HCID 22730282HCID 22730282, 화합물

시약·촉매·용매 6

HCID 142844-(Dimethylamino)pyridine
촉매
HCID 887Methanol용매
HCID 962Water용매
HCID 63651,1-Dichloroethane용매
HCID 8028Tetrahydrofuran용매
HCID 8857Ethyl Acetate용매

실험 절차

A mixture of Example 455B (1 g, 3.1 mmol) and LiOH (0-264 mg 6.2 mmol) in THF (15 mL), methanol (2.5 mL), and water (1.5 mL) was heated to 50° C. for 3 hours and concentrated. The concentrate was dissolved in DMF (10 mL) and treated with a mixture of Example 77B (1.059 g, 3 mmol), EDCI (1.146 g, 6 mmol), and DMAP (1.830, 15 mmol) in dichloroethane (10 mL), stirred for 16 hours, diluted with ethyl acetate (250 mL), washed sequentially with 1N HCl (50 mL, water (100 mL) and brine (100 mL), dried (MgSO4), filtered, and concentrated. The concentrate was purified by flash column chromatography on silica gel with 5% methanol/dichloromethane to provide the desired product. MS (ESI(−)) m/e 637 (M−H)−; 1H NMR (300 MHz, DMSO-d6) δ 8.78 (br t, 1H), 8.60 (d, 1H), 7.92 (dd, 1H), 7.85 (d, 2H), 7.55 (d, 2H), 7.40-7.15 (m, 6H), 6.35 (m, 1H), 4.21 (d, 2H), 3.65 (m, 2H), 3.52 (t, 2H), 3.25 (m, 4H), 1.45 (s, 9H).

후처리

  1. concentrationconcentrated
  2. dissolutionThe concentrate was dissolved in DMF (10 mL)
  3. washwashed sequentially with 1N HCl (50 mL, water (100 mL) and brine (100 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe concentrate was purified by flash column chromatography on silica gel with 5% methanol/dichloromethane

출처 및 근거

ORD 기록
ord-1d3ced85df9943319db3696667881c24
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07754886B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트