Hydrochloric Acid → HCID 19426302、化合物

HRID 2210295ノート

反応式

HRID 2210295 の反応式
[ClH:1].C(OC([N:9]1[CH2:14][CH2:13][CH:12]([OH:15])[CH:11]([N:16]2[CH2:21][CH2:20][C:19]3([C:30]4[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=4)[CH2:24][CH2:23][CH2:22]3)[CH2:18][CH2:17]2)[CH2:10]1)=O)(C)(C)C>CCOC(C)=O>[ClH:1].[ClH:1].[OH:15][CH:12]1[CH2:13][CH2:14][NH:9][CH2:10][CH:11]1[N:16]1[CH2:21][CH2:20][C:19]2([C:30]3[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH2:24][CH2:23][CH2:22]2)[CH2:18][CH2:17]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 104536361'-(1-t-butoxycarbonyl-4-hydroxypiperidin-3-yl)-3,4-dihydro-spiro[naphthalene-1(2H),4'-piperidine]

生成物 1

HCID 19426302HCID 19426302、化合物収率 80%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

HCl gas was bubbled for 30 min through a soln of 20c (800 mg, 2.1 mmol) in EtOAc (10 mL) while the flask was maintained in an ice bath. The resulting solution was subsequently stirred at room temperature for 30 min, and the volatiles were removed under reduced pressure. The white solid thus obtained was recrystallized from 50% isopropyl alcohol-hexanes to provide the hydrochlorides of 21c as a white powder (80%). Elemental analysis: Calc: C=61.12, H=8.1, N=7.5; Fnd: C=59.96, H=Elemental analysis: Gale: C=61.12, H=8.1, N=7.5; Fnd: C=59.96, H=7.95, N=6.86.

後処理

  1. temperaturewas maintained in an ice bath
  2. customthe volatiles were removed under reduced pressure
  3. customThe white solid thus obtained
  4. customwas recrystallized from 50% isopropyl alcohol-hexanes

出典と根拠

ORDレコード
ord-dfe0ae88f8fe456eb7515451ac263bca
出典データセット
uspto-grants-1995_10
特許番号
US05457207

反応ノート

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