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

isobutyl P-(4-aminobut-2-yl)-P-methyl-phosphinate → (3-Amino-1-methyl-propyl)-methyl-phosphinic acid

HRID 865836
노트
인쇄 미리보기

반응식

HRID 865836 반응식
[NH2:1][CH2:2][CH2:3][CH:4]([P:6]([CH3:13])(=[O:12])[O:7]CC(C)C)[CH3:5]>Cl>[NH2:1][CH2:2][CH2:3][CH:4]([P:6]([CH3:13])(=[O:7])[OH:12])[CH3:5]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 1

HCID 23374771isobutyl P-(4-aminobut-2-yl)-P-methyl-phosphinate

생성물 1

HCID 10219532(3-Amino-1-methyl-propyl)-methyl-phosphinic acid

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

A solution of 21.5 g of isobutyl P-(4-aminobut-2-yl)-P-methyl-phosphinate in 80 ml of 36% aqueous hydrochloric acid is heated to reflux for a period of 10 hours. The reaction mixture is then allowed to cool to room temperature, concentrated under reduced pressure, and co-evaporated twice with 100 ml of water. The crude material is dissolved in water, washed with chloroform, and the aqueous layer treated with activated charcoal. The aqueous solution is filtered hot, evaporated to dryness, the crude product is dissolved in 50 ml of methanol and treated with 1-2 ml of propylene oxide. The hygroscopic solid is filtered and triturated with acetone. After drying, P-(4-aminobut-2-yl)-P-methyl-phosphinic acid is obtained as a hygroscopic solid, m.p. 68°-75°, 3P-NMR spectrum: δ=+46.5 ppm (D2O).

후처리

  1. temperatureto reflux for a period of 10 hours
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe crude material is dissolved in water
  4. washwashed with chloroform
  5. additionthe aqueous layer treated with activated charcoal
  6. filtrationThe aqueous solution is filtered hot
  7. customevaporated to dryness
  8. dissolutionthe crude product is dissolved in 50 ml of methanol
  9. additiontreated with 1-2 ml of propylene oxide
  10. filtrationThe hygroscopic solid is filtered
  11. customtriturated with acetone
  12. customAfter drying

출처 및 근거

ORD 기록
ord-068af91a39184c53838690b3caaa0cc8
출처 데이터셋
uspto-grants-1996_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05567840

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트