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

Potassium Hydroxide → HCID 67327945, 화합물

HRID 1846144
노트
인쇄 미리보기

반응식

HRID 1846144 반응식
CC1[N:3]([C:8]2[N:13]=[C:12]([CH3:14])[C:11]([O:15][CH2:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)=[C:10]([CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][O:33][CH2:34][C:35]3[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=3)[N:9]=2)C(C)=CC=1.Cl.NO.[OH-].[K+].[OH-].[Na+]>C(O)C.O.O>[NH2:3][C:8]1[N:13]=[C:12]([CH3:14])[C:11]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)=[C:10]([CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][O:33][CH2:34][C:35]2[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=2)[N:9]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 14797Potassium HydroxideHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochloride2회HCID 67355138HCID 67355138, 화합물

생성물 1

HCID 67327945HCID 67327945, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 19096565
Water ethanol
용매

실험 절차

To stirred solution containing 343 mg (0.63 mmol) of 2-(2,5-dimethyl-1H-pyrrol-1-yl)-5-benzyloxy-4-methyl-6-(10-benzyloxydecyl)-pyrimidine (7) in 10 mL of ethanol-water 9:1 were added 500 mg (7.19 mmol) of hydroxylamine hydrochloride followed by 400 mg (7.14 mmol) of potassium hydroxide. The reaction mixture was then stirred at reflux under argon atmosphere overnight. A second portion of 500 mg (7.19 mmol) of hydroxylamine hydrochloride was added and the reaction mixture was stirred overnight at reflux under argon atmosphere. The reaction mixture was then poured into 70 mL of water and then basified to a pH 9-10 with a 1N NaOH solution. The mixture was extracted with two portions of 70 mL of dichloromethane. The combined organic solution was washed with a portion of 70 mL of brine, dried (MgSO4) and then concentrated under diminished pressure. The residue was purified by chromatography on a silica gel column. Elution with acetone-hexanes 2:1 gave the expected product as a colorless oil: yield 153 mg (52%). 1H-NMR (CDCl3) δ 7.48-7.37 (m, 10H), 5.17 (br., 2H), 4.69 (s, 2H), 4.45 (s, 2H), 3.41 (t, 2H, J=6.8), 2.55 (t, 2H, J=7.6), 2.26 (s, 3H), 1.63-1.53 (m, 4H), 1.27 (m, 12H); 13C-NMR (CDCl3) δ 164.85, 161.14, 158.88, 142.81, 138.71, 136.77, 129.16, 128.59, 128.26, 75.91, 72.83, 70.50, 31.90, 29.77, 29.22, 29.55, 29.45, 29.41, 28.44, 28.19, 19.00.

후처리

  1. stirringThe reaction mixture was then stirred
  2. temperatureat reflux under argon atmosphere overnight
  3. stirringthe reaction mixture was stirred overnight
  4. temperatureat reflux under argon atmosphere
  5. extractionThe mixture was extracted with two portions of 70 mL of dichloromethane
  6. washThe combined organic solution was washed with a portion of 70 mL of brine
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated under diminished pressure
  9. customThe residue was purified by chromatography on a silica gel column
  10. washElution with acetone-hexanes 2:1

출처 및 근거

ORD 기록
ord-328517402a954e9bab0b1e747dcd64db
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08952025B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트