Hydrochloric Acid → (2S,4S)-1-(2-(1H-1,2,4-triazol-1-yl)acetyl)-4-aminomethyl-N-(4-(4-fluorophenoxy)phenyl)pyrrolidine-2-carboxamide hydrochloride salt

HRID 1630085

반응식

HRID 1630085 반응식
[N:1]1([CH2:6][C:7]([N:9]2[CH2:13][C@H:12]([C:14]#[N:15])[CH2:11][C@H:10]2[C:16]([NH:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][C:26]3[CH:31]=[CH:30][C:29]([F:32])=[CH:28][CH:27]=3)=[CH:21][CH:20]=2)=[O:17])=[O:8])[CH:5]=[N:4][CH:3]=[N:2]1.[ClH:33]>[Pd].CO>[ClH:33].[N:1]1([CH2:6][C:7]([N:9]2[CH2:13][C@H:12]([CH2:14][NH2:15])[CH2:11][C@H:10]2[C:16]([NH:18][C:19]2[CH:24]=[CH:23][C:22]([O:25][C:26]3[CH:27]=[CH:28][C:29]([F:32])=[CH:30][CH:31]=3)=[CH:21][CH:20]=2)=[O:17])=[O:8])[CH:5]=[N:4][CH:3]=[N:2]1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 67010058(2S,4R)-1-(2-(1H-1,2,4-triazol-1-yl)acetyl)-4-cyano-N-(4-(4-fluorophenoxy)phenyl)pyrrolidine-2-carboxamide

생성물 1

HCID 67010106(2S,4S)-1-(2-(1H-1,2,4-triazol-1-yl)acetyl)-4-aminomethyl-N-(4-(4-fluorophenoxy)phenyl)pyrrolidine-2-carboxamide hydrochloride salt수율 94.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A flask was charged with (2S,4R)-1-(2-(1H-1,2,4-triazol-1-yl)acetyl)-4-cyano-N-(4-(4-fluorophenoxy)phenyl)pyrrolidine-2-carboxamide (260 mg, 0.599 mmol), prepared as in Reference 11, methanol (4 mL), hydrogen chloride (4N in dioxane, 16 mmol) and palladium on carbon (10%, 100 mg) and the mixture was placed under a hydrogen atmosphere (balloon). The mixture was stirred for 18 hours at ambient temperature, filtered and concentrated to give crude (2S,4S)-1-(2-(1H-1,2,4-triazol-1-yl)acetyl)-4-aminomethyl-N-(4-(4-fluorophenoxy)phenyl)pyrrolidine-2-carboxamide hydrochloride salt (0.247 g, 0.564 mmol).

후처리

  1. filtrationfiltered
  2. concentrationconcentrated

출처 및 근거

ORD 기록
ord-e72b53e2622e451e906ea0a278078dac
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08791102B2

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