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

Sodium Hydroxide → HCID 178494614, 화합물

HRID 1871537
노트
인쇄 미리보기

반응식

HRID 1871537 반응식
[CH:1]1([O:6][C:7]2[CH:8]=[C:9]([CH:19]=[CH:20][C:21]=2[O:22][CH3:23])[CH2:10][NH:11][C:12]2[C:16]([CH2:17][OH:18])=[CH:15][NH:14][N:13]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1.O.[C:25]1(C)C=CC(S(O)(=O)=O)=CC=1.[OH-].[Na+]>CO>[CH:1]1([O:6][C:7]2[CH:8]=[C:9]([CH:19]=[CH:20][C:21]=2[O:22][CH3:23])[CH2:10][NH:11][C:12]2[C:16]([CH2:17][O:18][CH3:25])=[CH:15][NH:14][N:13]=2)[CH2:5][CH2:4][CH2:3][CH2:2]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 521998p-Toluenesulfonic acid monohydrateHCID 1784910433-(3-Cyclopentyloxy-4-methoxybenzylamino)-4-hydroxymethylpyrazole

생성물 1

HCID 178494614HCID 178494614, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 3-(3-cyclopentyloxy-4-methoxybenzylamino)-4-hydroxymethylpyrazole (1.0 g, 3.15 mmol) and p-toluenesulfonic acid monohydrate (0.2 g, 1.0 mmol) in methanol (100 mL) was kept at room temperature for 10 min. The reaction mixture was neutralized with 1 N aqueous sodium hydroxide and evaporated under reduced pressure at room temperature. The residue was partitioned between water (50 mL) and ethyl acetate (50 mL). The layers were separated and the aqueous layer was extracted with ethyl acetate (10 mL). The combined ethyl acetate layers were washed with water and evaporated under reduced pressure. The residue was taken up in a small volume of methylene chloride and applied to a 4 mm silica gel disk on a Chromatotron. Elution with 525 mL of methylene chloride and 275 mL of 1% methanol/methylene chloride removed some impure material. Continued elution with 75 mL of 1% methanol/methylene chloride afforded 380 mg (36%) of pure 3-(3-cyclopentyloxy-4-methoxybenzylamino)-4-methyoxymethylpurazole, mp. 112-115°.

후처리

  1. customevaporated under reduced pressure at room temperature
  2. customThe residue was partitioned between water (50 mL) and ethyl acetate (50 mL)
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with ethyl acetate (10 mL)
  5. washThe combined ethyl acetate layers were washed with water
  6. customevaporated under reduced pressure
  7. washElution with 525 mL of methylene chloride and 275 mL of 1% methanol/methylene chloride
  8. customremoved some impure material
  9. washelution with 75 mL of 1% methanol/methylene chloride
  10. customafforded 380 mg (36%) of pure 3-(3-cyclopentyloxy-4-methoxybenzylamino)-4-methyoxymethylpurazole, mp. 112-115°

출처 및 근거

ORD 기록
ord-08b0017829594762a81f73aa601ebb61
출처 데이터셋
uspto-grants-2000_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06103749

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트