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

1,2-Dichloroethane → N-[(1S,2S)-2-{[3-Ethyl-5-(trifluoromethyl)pyrazin-2-yl]amino}cyclopentyl]-5-fluoro-2-(pyrimidin-2-yl)benzamide

HRID 1750716
노트
인쇄 미리보기

반응식

HRID 1750716 반응식
[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:11]2[N:16]=[CH:15][CH:14]=[CH:13][N:12]=2)=[C:6]([CH:10]=1)[C:7]([OH:9])=O.N1C2C(=NC=CC=2)N(O)N=1.C(Cl)CCl.C(N(CC)CC)C.Cl.[CH2:39]([C:41]1[C:42]([NH:51][C@H:52]2[CH2:56][CH2:55][CH2:54][C@@H:53]2[NH2:57])=[N:43][CH:44]=[C:45]([C:47]([F:50])([F:49])[F:48])[N:46]=1)[CH3:40]>C(Cl)Cl>[CH2:39]([C:41]1[C:42]([NH:51][C@H:52]2[CH2:56][CH2:55][CH2:54][C@@H:53]2[NH:57][C:7](=[O:9])[C:6]2[CH:10]=[C:2]([F:1])[CH:3]=[CH:4][C:5]=2[C:11]2[N:16]=[CH:15][CH:14]=[CH:13][N:12]=2)=[N:43][CH:44]=[C:45]([C:47]([F:50])([F:48])[F:49])[N:46]=1)[CH3:40]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 181649HOAtHCID 670869505-Fluoro-2-(pyrimidin-2-yl)benzoic acidHCID 118308132(1S,2S)-1-N-[3-Ethyl-5-(trifluoromethyl)pyrazin-2-yl]cyclopentane-1,2-diamine hydrochloride2회

생성물 1

HCID 91827608
N-[(1S,2S)-2-{[3-Ethyl-5-(trifluoromethyl)pyrazin-2-yl]amino}cyclopentyl]-5-fluoro-2-(pyrimidin-2-yl)benzamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 5-fluoro-2-(pyrimidin-2-yl)benzoic acid (CAS number 1293284-57-7; 53 mg, 0.24 mmol), 3H-[1,2,3]triazolo[4,5-b]pyridin-3-ol (33 mg, 0.24 mmol), EDC (46.3 mg, 0.241 mmol) and triethylamine (0.067 ml, 0.48 mmol) in DCM (5 ml) was added (1S,2S)-1-N-[3-ethyl-5-(trifluoromethyl)pyrazin-2-yl]cyclopentane-1,2-diamine hydrochloride (Intermediate 41; 50 mg, 0.161 mmol). The reaction mixture was stirred at room temperature for 88 hours and then partitioned between DCM and a saturated solution of sodium bicarbonate, passing through a hydrophobic frit. The organics were loaded directly on to a cation/anion mixed mode cartridge, eluted with DCM and concentrated in vacuo. This was then purified by reverse phase chromatography (C18 silica, 0-100% acetonitrile/water with 0.1% ammonia). The resulting aqueous was concentrated in vacuo and extracted with DCM. The organics were concentrated in vacuo to afford the title compound.

후처리

  1. custompartitioned between DCM
  2. additionmixed mode cartridge
  3. washeluted with DCM
  4. concentrationconcentrated in vacuo
  5. customThis was then purified by reverse phase chromatography (C18 silica, 0-100% acetonitrile/water with 0.1% ammonia)
  6. concentrationThe resulting aqueous was concentrated in vacuo
  7. extractionextracted with DCM
  8. concentrationThe organics were concentrated in vacuo

출처 및 근거

ORD 기록
ord-c3375234c59d46b38d9fa1a892e22a3f
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09156829B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트