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

Sodium Bicarbonate → HCID 178433787, 화합물

HRID 384360
노트
인쇄 미리보기

반응식

HRID 384360 반응식
[OH:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([C:15]2[NH:16][CH2:17][CH2:18][N:19]=2)=[CH:11][CH:10]=1.[N:20]([O-])=O.[Na+].[CH2:24]1[C:32]2[C:27](=[CH:28][C:29]([N:33]3[C:37](=[O:38])[CH2:36][C:35]([CH3:39])=[N:34]3)=[CH:30][CH:31]=2)[CH2:26][CH2:25]1.C(=O)(O)[O-].[Na+]>Cl.C(O)C>[NH:19]1[CH2:18][CH2:17][N:16]=[C:15]1[C:12]1[CH:11]=[CH:10][C:9]([C:3]2[CH:4]=[CH:5][CH:6]=[C:7]([NH:8][N:20]=[C:36]3[C:35]([CH3:39])=[N:34][N:33]([C:29]4[CH:28]=[C:27]5[C:32](=[CH:31][CH:30]=4)[CH2:24][CH2:25][CH2:26]5)[C:37]3=[O:38])[C:2]=2[OH:1])=[CH:14][CH:13]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 516892Sodium BicarbonateHCID 23668193Sodium NitriteHCID 574837802-Indan-5-yl-5-methyl-2,4-dihydro-pyrazol-3-oneHCID 136006496HCID 136006496, 화합물

생성물 1

HCID 178433787HCID 178433787, 화합물수율 30.3%

시약·촉매·용매 2

HCID 313
Hydrochloric Acid
용매
HCID 702Ethanol용매

실험 절차

2-(2′-Hydroxy-3′-amino-biphenyl-4-yl-4,5-dihydro-1H-imidazol 32d (334 mg, 1.11 mmol) was dissolved in hydrochloric acid (3.7 mL, 1 mol/L) upon cooling by an ice-water bath, followed by dropwise addition of 1.5 mL of aqueous sodium nitrite (85 mg, 1.22 mmol). After the mixture was reacted for 20 minutes, 2-indan-5-yl-5-methyl-2,4-dihydro-pyrazol-3-one 1i (214 mg, 1 mmol) was added. The mixture was adjusted to pH 8 with saturated aqueous sodium bicarbonate, followed by addition of 5 mL of ethanol. The reaction mixture was reacted overnight at room temperature. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was filtered and 30 mL of water was added to the filter cake. After mixing well, the mixture was adjusted to pH 4 with concentrated hydrochloric acid to form precipitates. The mixture was filtered and the filter cake was purified by silica gel column chromatography to obtain the title compound 4-{[4′-(4,5-dihydro-1H-imidazol-2-yl)-2-hydroxy-biphenyl-3-yl]-hydrazono}-2-indan-5-yl-5-methyl-2,4-dihydro-pyrazol-3-one 32 (145 mg, yield 30.3%) as a red solid.

후처리

  1. temperatureupon cooling by an ice-water bath
  2. customAfter the mixture was reacted for 20 minutes
  3. customThe reaction mixture was reacted overnight at room temperature
  4. filtrationThe mixture was filtered
  5. addition30 mL of water was added to the filter cake
  6. additionAfter mixing well
  7. customto form
  8. customprecipitates
  9. filtrationThe mixture was filtered
  10. customthe filter cake was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-5e0fba0ec4974344b00d926f864ea9fc
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08367710B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트