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

Hydrochloric Acid → HCID 178515380, 화합물

HRID 1096912
노트
인쇄 미리보기

반응식

HRID 1096912 반응식
[CH:1]1([C:4]2[N:8]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)[C:7]3[CH:15]=[CH:16][C:17]([C:19](OC)=[O:20])=[CH:18][C:6]=3[N:5]=2)[CH2:3][CH2:2]1.[OH-].[Na+].Cl.Cl.[NH:27]1[C:31]([C:32]2[CH:33]=[C:34]3[C:44](=[CH:45][CH:46]=2)[O:43][C:37]2([CH2:42][CH2:41][NH:40][CH2:39][CH2:38]2)[CH2:36][C:35]3=[O:47])=[N:30][N:29]=[N:28]1.C(N(CC)CC)C.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl>C1COCC1.CO.O.CN(C=O)C>[CH:1]1([C:4]2[N:8]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)[C:7]3[CH:15]=[CH:16][C:17]([C:19]([N:40]4[CH2:41][CH2:42][C:37]5([CH2:36][C:35](=[O:47])[C:34]6[C:44](=[CH:45][CH:46]=[C:32]([C:31]7[NH:27][N:28]=[N:29][N:30]=7)[CH:33]=6)[O:43]5)[CH2:38][CH2:39]4)=[O:20])=[CH:18][C:6]=3[N:5]=2)[CH2:3][CH2:2]1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

12

반응물 7

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 66782575HCID 66782575, 화합물HCID 178479612HCID 178479612, 화합물

생성물 1

HCID 178515380HCID 178515380, 화합물

시약·촉매·용매 4

HCID 887Methanol용매HCID 962Water용매2회HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
60 °C

실험 절차

Methyl 2-cyclopropyl-1-phenyl-1H-benzimidazole-5-carboxylate (194 mg, 0.664 mmol) was dissolved in THF (6 mL) and MeOH (6 mL), and aqueous 5 N sodium hydroxide solution (0.66 mL, 3.30 mmol) was added to it and stirred at 60° C. for 2 hours. This was restored to room temperature, 5 N hydrochloric acid (0.66 mL, 3.30 mmol) was added thereto, the solvent was evaporated away under reduced pressure, and the residue was azeotroped with toluene. DMF (4 mL) and water (1 mL) were added to it, and 6-(tetrazol-5-yl)spiro[chroman-2,4′-piperidin]-4-one hydrochloride (256 mg, 0.797 mmol), triethylamine (0.14 mL, 0.996 mmol), HOBT (135 mg, 0.996 mmol) and WSC hydrochloride (191 mg, 0.996 mmol) were added thereto. The reaction liquid was stirred at 90° C. for 2 hours, restored to room temperature, and water was added thereto. The precipitated solid was taken out through filtration, and dried under reduced pressure to obtain the title compound as a white solid. 1H-NMR (400 MHz, DMSO-d6) δ: 8.42 (1H, d, J=2.2 Hz), 8.23 (1H, dd, J=8.8, 2.2 Hz), 7.69-7.59 (6H, m), 7.34 (1H, d, J=8.8 Hz), 7.23 (1H, dd, J=8.4, 1.6 Hz), 7.14 (1H, d, J=8.4 Hz), 4.50-3.29 (5H, m), 2.98 (2H, s), 2.06-1.77 (4H, m), 1.15-1.11 (2H, m), 1.04-1.00 (2H, m). MS [M+H]+=546.

후처리

  1. customThis was restored to room temperature
  2. customthe solvent was evaporated away under reduced pressure
  3. customthe residue was azeotroped with toluene
  4. additionwere added
  5. customThe reaction liquid
  6. stirringwas stirred at 90° C. for 2 hours
  7. customrestored to room temperature
  8. filtrationThe precipitated solid was taken out through filtration
  9. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-1fbf4ef97e74427981522cd036cbf70e
출처 데이터셋
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08138197B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트