Hydrochloric Acid → HCID 66877304、化合物

HRID 1993872ノート

反応式

HRID 1993872 の反応式
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

参加物

5

反応物 3

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

生成物 1

HCID 66877304HCID 66877304、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-40d13ccc93ed474096ae4f646685e45f
出典データセット
uspto-grants-2010_01
特許番号
US07652053B2

反応ノート

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