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

2-Dibenzylamino-1,1-dimethylethylamine → 3-(2-Amino-1,1-dimethylethylamino)-1-(3-methylbenzimidazol-4-yloxy)-propan-2-ol

HRID 1607127
노트
인쇄 미리보기

반응식

HRID 1607127 반응식
[O:1]1[CH2:15][CH:2]1[CH2:3][O:4][C:5]1[C:13]2[N:12]([CH3:14])[CH:11]=[N:10][C:9]=2[CH:8]=[CH:7][CH:6]=1.C([N:23](CC1C=CC=CC=1)[CH2:24][C:25]([NH2:28])([CH3:27])[CH3:26])C1C=CC=CC=1.[H][H]>[Pd].C(O)C>[NH2:23][CH2:24][C:25]([NH:28][CH2:15][CH:2]([OH:1])[CH2:3][O:4][C:5]1[C:13]2[N:12]([CH3:14])[CH:11]=[N:10][C:9]=2[CH:8]=[CH:7][CH:6]=1)([CH3:27])[CH3:26]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 117778302-Dibenzylamino-1,1-dimethylethylamineHCID 198530372,3-Epoxy-1-(3-methylbenzimidazol-4-yloxy)-propaneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 198529363-(2-Amino-1,1-dimethylethylamino)-1-(3-methylbenzimidazol-4-yloxy)-propan-2-ol

시약·촉매·용매 2

HCID 23938Palladium촉매
HCID 702
Ethanol
용매

실험 절차

10.2 g. 2,3-Epoxy-1-(3-methylbenzimidazol-4-yloxy)-propane are added to 40.3 g. 2-dibenzylamino-1,1-dimethylethylamine (prepared analogously to H. G. Johnson, J.A.C.S., 68, 12/1946) in 300 ml. ethanol and the reaction mixture is stirred for 3 days at ambient temperature. The reaction mixture is now hydrogenated at 60° C. over 8 g. palladium-charcoal (10%) until the take up of hydrogen is finished. The catalyst is then filtered off with suction and the filtrate evaporated to dryness. The residue is chromatographed on silica gel with methanol/concentrated aqueous ammonia solution (95:5 v/v). The appropriate fractions are evaporated, the residue is taken up in methylene chloride and dried over anhydrous sodium sulphate and the solution is evaporated to dryness. There are obtained 8.7 g. (66% of theory) of the desired product as a pale yellow oil.

후처리

  1. customis now hydrogenated at 60° C. over 8 g
  2. filtrationThe catalyst is then filtered off with suction
  3. customthe filtrate evaporated to dryness
  4. customThe residue is chromatographed on silica gel with methanol/concentrated aqueous ammonia solution (95:5 v/v)
  5. customThe appropriate fractions are evaporated
  6. dry with materialdried over anhydrous sodium sulphate
  7. customthe solution is evaporated to dryness
  8. customThere are obtained 8.7 g

출처 및 근거

ORD 기록
ord-a57c0b9d57564d44bb79d1de126609cf
출처 데이터셋
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04863949

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트