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

Ethyl Acetate → HCID 178433731, 화합물

HRID 1909060
노트
인쇄 미리보기

반응식

HRID 1909060 반응식
CN(C[N:5]1[C:9]2=[N:10][C:11]([N:14]3[CH2:19][CH2:18][CH:17]([N:20]([CH3:22])[CH3:21])[CH2:16][CH2:15]3)=[CH:12][CH:13]=[C:8]2[N:7]=[CH:6]1)C.C(NC(C)C)(C)C.[Li].C[O:32][C:33](=O)[C:34]1[CH:39]=[CH:38][C:37]([C:40]#[N:41])=[C:36]([C:42]2[C:46]([CH3:47])=[N:45][N:44]3[CH2:48][CH2:49][CH2:50][C:43]=23)[CH:35]=1.CCOC(C)=O>C1COCC1>[CH3:22][N:20]([CH3:21])[CH:17]1[CH2:16][CH2:15][N:14]([C:11]2[N:10]=[C:9]3[NH:5][C:6]([C:33]([C:34]4[CH:39]=[CH:38][C:37]([C:40]#[N:41])=[C:36]([C:42]5[C:46]([CH3:47])=[N:45][N:44]6[CH2:48][CH2:49][CH2:50][C:43]=56)[CH:35]=4)=[O:32])=[N:7][C:8]3=[CH:13][CH:12]=2)[CH2:19][CH2:18]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8857Ethyl AcetateHCID 45051747Lithium diisopropylamineHCID 66599667[1-(3-dimethylaminomethyl-3H-imidazo[4,5-b]pyridin-5-yl)-piperidin-4-yl]-dimethyl-amineHCID 66599721HCID 66599721, 화합물

생성물 1

HCID 178433731HCID 178433731, 화합물수율 10%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
3회

반응 조건

온도
-78 °C

실험 절차

To a solution of [1-(3-dimethylaminomethyl-3H-imidazo[4,5-b]pyridin-5-yl)-piperidin-4-yl]-dimethyl-amine (0.36 g, 1.2 mmol) in THF (5 mL) at −78° C. under N2 was added dropwise a freshly prepared solution of lithium diisopropylamine (1M, 1.5 mL, 1.5 mmol) in THF. After 10 m at −78° C. a solution of 4-cyano-3-(2-methyl-5,6-dihydro-4H-pyrrolo[1,2-b]pyrazol-3-yl)-benzoic acid methyl ester (0.28 g, 1.0 mmol) in THF (5 mL) was added. The reaction mixture was stirred at −78° C. under N2 for 15 m before quenching with a 1:1 solution of acetic acid and water (2 mL). After warming to room temperature the quenched reaction was diluted several fold EtOAc and washed with dilute NH4OH followed by brine. The organic layer was dried over Na2SO4, filtered and concentrated. After purifying the crude product by reverse phase HPLC, the product was neutralized with aqueous Na2CO3 yielding the desired product as a orange-colored solid (50 mg, 0.10 mmol). 1H NMR (400 MHz, DMSO-d6) □ ppm 1.32-1.44 (m, J=12.00, 11.81, 11.81, 3.79 Hz, 2H) 1.85 (d, J=10.61 Hz, 2H) 2.20 (s, 6H) 2.25 (s, 3H) 2.33-2.46 (m, 1H) 2.53-2.63 (m, 2H) 2.89-3.02 (m, 4H) 4.43 (d, J=13.14 Hz, 2H) 7.04 (d, J=9.09 Hz, 1H) 7.95 (d, J=9.09 Hz, 1H) 8.10 (d, J=8.08 Hz, 1H) 8.36 (d, J=7.58 Hz, 1H) 8.52 (s, 1H); MS m/z 495.5 (M+H)+.

후처리

  1. custombefore quenching with a 1:1 solution of acetic acid and water (2 mL)
  2. temperatureAfter warming to room temperature
  3. customthe quenched reaction
  4. washwashed with dilute NH4OH
  5. dry with materialThe organic layer was dried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customAfter purifying the crude product by reverse phase HPLC

출처 및 근거

ORD 기록
ord-d2e0f81039e14b6b8378f55b6c401c1a
출처 데이터셋
uspto-grants-2013_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08598217B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트