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

Acetic Acid → HCID 178481783, 화합물

HRID 931211
노트
인쇄 미리보기

반응식

HRID 931211 반응식
[CH3:1][N:2]1[C:6]([CH2:7][C:8]#[N:9])=[CH:5][CH:4]=[N:3]1.[C:10](Cl)(=O)[CH3:11].Cl.Cl.N[C:17]1[CH:18]=[CH:19][C:20]([N:24]2[CH2:29][CH2:28][CH2:27][C@@H:26]([C:30]([N:32]3[CH2:36][CH2:35][CH2:34][CH2:33]3)=[O:31])[CH2:25]2)=[N:21][C:22]=1[NH2:23].C(N(CC)CC)C.C(O)(=O)C>C(O)C>[CH3:1][N:2]1[C:6]([C:7]2([C:8]3[NH:23][C:22]4=[N:21][C:20]([N:24]5[CH2:29][CH2:28][CH2:27][C@@H:26]([C:30]([N:32]6[CH2:36][CH2:35][CH2:34][CH2:33]6)=[O:31])[CH2:25]5)=[CH:19][CH:18]=[C:17]4[N:9]=3)[CH2:11][CH2:10]2)=[CH:5][CH:4]=[N:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 176Acetic AcidHCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 252483742-(1-methyl-1H-pyrazol-5-yl)acetonitrileHCID 89854051(R)-(1-(5,6-Diaminopyridin-2-yl)piperidin-3-yl)(pyrrolidin-1-yl)methanone dihydrochloride

생성물 1

HCID 178481783HCID 178481783, 화합물

시약·촉매·용매

1
HCID 702Ethanol용매2회

실험 절차

To a solution of 2-(1-methyl-1H-pyrazol-5-yl)acetonitrile (14.5 mg, 0.10 mmol) in ethanol (150 μL, 2.6 mmol) was added acetyl chloride (110 μL, 1.5 mmol). The reaction mixture was stirred at room temperature for 16 h. The solvent was removed under a stream of nitrogen. Ethanol (0.5 mL) was added to the residue followed by a solution of (R)-(1-(5,6-diaminopyridin-2-yl)piperidin-3-yl)(pyrrolidin-1-yl)methanone dihydrochloride (36 mg, 0.01 mmol) and triethylamine (70 μL, 0.50 mmol) in ethanol (1 mL). Acetic acid (100 μL, 1.75 mmol) was added and the reaction mixture was heated in the microwave for 45 min at 130° C. The solvent was removed under a stream of nitrogen. Ethyl acetate (10 mL) was added to the residue. The solution was washed with aqueous sodium hydroxide (1N, 3 mL), washed with water (3 mL), washed with brine (3 mL), dried over magnesium sulfate, filtered and concentrated under reduced pressure. The crude material was purified via HPLC to afford the title compound. MS (ESI+) (M+H) 420.3; HPLC retention time 1.88 min (Method B).

후처리

  1. customThe solvent was removed under a stream of nitrogen
  2. additionEthanol (0.5 mL) was added to the residue
  3. temperaturethe reaction mixture was heated in the microwave for 45 min at 130° C
  4. customThe solvent was removed under a stream of nitrogen
  5. additionEthyl acetate (10 mL) was added to the residue
  6. washThe solution was washed with aqueous sodium hydroxide (1N, 3 mL)
  7. washwashed with water (3 mL)
  8. washwashed with brine (3 mL)
  9. dry with materialdried over magnesium sulfate
  10. filtrationfiltered
  11. concentrationconcentrated under reduced pressure
  12. customThe crude material was purified via HPLC

출처 및 근거

ORD 기록
ord-061c00ae9b70407cb3b1423857ec3dce
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09296745B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트