Hydrochloric Acid → HCID 66877304, 화합물

HRID 1993872노트

반응식

HRID 1993872 반응식
C(OC(=O)[NH:7][C@H:8]1[CH2:12][CH2:11][C@H:10]([N:13]2[C:17]3[CH:18]=[CH:19][C:20]([CH3:22])=[CH:21][C:16]=3[N:15]=[C:14]2[CH3:23])[CH2:9]1)(C)(C)C.CO.[ClH:27]>O1CCOCC1>[ClH:27].[CH3:23][C:14]1[N:13]([C@H:10]2[CH2:11][CH2:12][C@H:8]([NH2:7])[CH2:9]2)[C:17]2[CH:18]=[CH:19][C:20]([CH3:22])=[CH:21][C:16]=2[N:15]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 66877180trans-[3-(2,5-Dimethyl-benzoimidazol-1-yl)-cyclopentyl]-carbamic acid tert-butyl ester

생성물 1

HCID 66877304HCID 66877304, 화합물

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

The trans-[3-(2,5-dimethyl-benzoimidazol-1-yl)-cyclopentyl]-carbamic acid tert-butyl ester prepared above (320 mg, 0.95 mmol) was dissolved in HCl (4M) in dioxane (5.0 mL) and the solution was stirred for 15 minutes. Solids came out of solution and 1 mL of methanol was added to dissolve the precipitate. Stirring was continued for 60 minutes and the reaction mixture was evaporated to a sticky solid which was stirred with ethyl ether. The resulting solid was filtered to provide trans-3-(2,5-dimethyl-benzoimidazol-1-yl)-cyclopentylamine hydrochloride salt as an off white powder (250 mg). LR-MS calcd for C14H19N3 (m/e) 229.1579, obsd 230.2 (M+H).

후처리

  1. additionwas added
  2. dissolutionto dissolve the precipitate
  3. stirringStirring
  4. waitwas continued for 60 minutes
  5. customthe reaction mixture was evaporated to a sticky solid which
  6. stirringwas stirred with ethyl ether
  7. filtrationThe resulting solid was filtered

출처 및 근거

ORD 기록
ord-40d13ccc93ed474096ae4f646685e45f
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07652053B2

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