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

Cyclohexylamine → HCID 25241920, 화합물

HRID 1852533
노트
인쇄 미리보기

반응식

HRID 1852533 반응식
[CH:1]1([NH2:7])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl[C:9]1[N:14]=[C:13]([N:15]2[C:19]3[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=3[N:17]=[N:16]2)[C:12]([Cl:24])=[CH:11][N:10]=1>C1COCC1>[N:15]1([C:13]2[C:12]([Cl:24])=[CH:11][N:10]=[C:9]([NH:7][CH:1]3[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]3)[N:14]=2)[C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[N:17]=[N:16]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7965CyclohexylamineHCID 25241964HCID 25241964, 화합물

생성물 1

HCID 25241920HCID 25241920, 화합물수율 53%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Cyclohexylamine (0.21 mL, 1.88 mmol) was added in portions to a solution of 1-(2,5-dichloro-pyrimidin-4-yl)-1H-benzotriazole (250 mg, 0.94 mmol) in THF (30 mL) at RT under nitrogen atmosphere. The resultant colorless solution was stirred at RT for 4 hours. TEA (2.82 mmol) was then added and the reaction mixture was stirred at RT overnight. The mixture was partitioned between water (50 mL) and EtOAc (50 mL). The organic layer was separated, washed twice with water (50 mL) and once with brine (50 mL), then dried over Na2SO4, filtered and evaporated under reduced pressure to give an off-white solid. This crude material was purified via flash chromatography (toluene/EtOAc, 98/2) to afford 162 mg (53% yield) of (4-benzotriazol-1-yl-5-chloro-pyrimidin-2-yl)-cyclohexyl-amine as an off-white solid. MS: 329.14 (M+1)+, 301.14 ((M+1)+−28).

후처리

  1. stirringthe reaction mixture was stirred at RT overnight
  2. customThe mixture was partitioned between water (50 mL) and EtOAc (50 mL)
  3. customThe organic layer was separated
  4. washwashed twice with water (50 mL) and once with brine (50 mL)
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. customevaporated under reduced pressure
  8. customto give an off-white solid
  9. customThis crude material was purified via flash chromatography (toluene/EtOAc, 98/2)

출처 및 근거

ORD 기록
ord-aad022192ca94a889345a591ca20975e
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08962622B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트