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Hydrochloric Acid → 5-Methoxy-6-chloro-8-methyl-1,2,3,3a,8,8a-hexahydroindeno[1,2-c]pyrrole

HRID 508497
ノート
印刷プレビュー

反応式

HRID 508497 の反応式
O.O.O.O.O.O.O.O.[OH-].[Ba+2].[OH-].C(NC(=O)[O-])C.[CH3:18][O:19][C:20]1[C:21]([Cl:33])=[CH:22][C:23]2[CH:24]([CH3:32])[CH:25]3[CH2:29][NH:28][CH2:27][CH:26]3[C:30]=2[CH:31]=1.Cl>CO>[CH3:18][O:19][C:20]1[C:21]([Cl:33])=[CH:22][C:23]2[CH:24]([CH3:32])[CH:25]3[CH2:29][NH:28][CH2:27][CH:26]3[C:30]=2[CH:31]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 17749109Barium hydroxide, octahydrateHCID 86602844N-Ethylcarbamate 5-methoxy-6-chloro-8-methyl-1,2,3,3a,8,8a-hexahydroindeno[1,2-c]pyrrole

生成物 1

HCID 117085025-Methoxy-6-chloro-8-methyl-1,2,3,3a,8,8a-hexahydroindeno[1,2-c]pyrrole

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Barium hydroxide octahydrate (0.63 g, 2.0 mmol) was added to a solution of N-ethylcarbamate-5-methoxy-6-chloro-8-methyl-1,2,3,3a,8,8a-hexahydroindeno[1,2-c]pyrrole (61 mg, 0.2 mmol) in MeOH (4 mL), and stirred for 24 hours at reflux. The reaction mixture was cooled to room temperature and neutralized to pH=7 with aqueous HCl (50 mL, 1 M). The product was extracted with CH2Cl2, dried over MgSO4, and concentrated. The crude product was purified by reverse-phase liquid chromatography to afford the title compound. MS calculated for C13H16ClNO+H: 238, observed: 238.

後処理

  1. temperatureat reflux
  2. extractionThe product was extracted with CH2Cl2
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated
  5. customThe crude product was purified by reverse-phase liquid chromatography

出典と根拠

ORDレコード
ord-7b2c1f7050154160b1598f2a3b3646ae
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09096520B2

反応ノート

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