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Hydrochloric Acid → N-[(4'R)-2''-amino-2',2'-dimethyldispiro[cyclopropane-1,3'-chromene-4',4''-[1,3]oxazol]-6'-yl]-5-(difluoromethyl)pyrazine-2-carboxamide hydrochloride

HRID 594919
ノート
印刷プレビュー

反応式

HRID 594919 の反応式
[NH2:1][C:2]1[O:3][CH2:4][C@@:5]2([C:15]3[C:10](=[CH:11][CH:12]=[C:13]([NH:16][C:17]([C:19]4[CH:24]=[N:23][C:22]([CH:25]([F:27])[F:26])=[CH:21][N:20]=4)=[O:18])[CH:14]=3)[O:9][C:8]([CH3:29])([CH3:28])[C:7]32[CH2:31][CH2:30]3)[N:6]=1.[ClH:32].C(OCC)(=O)C>CO>[ClH:32].[NH2:1][C:2]1[O:3][CH2:4][C@@:5]2([C:15]3[C:10](=[CH:11][CH:12]=[C:13]([NH:16][C:17]([C:19]4[CH:24]=[N:23][C:22]([CH:25]([F:27])[F:26])=[CH:21][N:20]=4)=[O:18])[CH:14]=3)[O:9][C:8]([CH3:29])([CH3:28])[C:7]32[CH2:31][CH2:30]3)[N:6]=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 8857Ethyl AcetateHCID 86724318N-[(4'R)-2''-amino-2',2'-dimethyldispiro[cyclopropane-1,3'-chromene-4',4''-[1,3]oxazol]-6'-yl]-5-(difluoromethyl)pyrazine-2-carboxamide

生成物 1

HCID 86724321N-[(4'R)-2''-amino-2',2'-dimethyldispiro[cyclopropane-1,3'-chromene-4',4''-[1,3]oxazol]-6'-yl]-5-(difluoromethyl)pyrazine-2-carboxamide hydrochloride

試薬・触媒・溶媒 1

HCID 887
Methanol
溶媒

実験手順

To a solution of N-[(4′R)-2″-amino-2′,2′-dimethyldispiro[cyclopropane-1,3′-chromene-4′,4″-[1,3]oxazol]-6′-yl]-5-(difluoromethyl)pyrazine-2-carboxamide (800 mg, 1.86 mmol) in MeOH (10 mL) was added 4M solution of hydrogen chloride in ethyl acetate (0.5 mL, 2 mmol) and the mixture was concentrated in vacuo. The residue was triturated with EtOH (10 mL), and the mixture was refluxed for 30 minutes and stirred at room temperature overnight. The precipitate was collected, washed with EtOH (2 mL), and dried under reduced pressure at 70° C. overnight to afford N-[(4′R)-2″-amino-2′,2′-dimethyldispiro[cyclopropane-1,3′-chromene-4′,4″-[1,3]oxazol]-6′-yl]-5-(difluoromethyl)pyrazine-2-carboxamide hydrochloride (449 mg) as a crystal.

後処理

  1. concentrationthe mixture was concentrated in vacuo
  2. customThe residue was triturated with EtOH (10 mL)
  3. temperaturethe mixture was refluxed for 30 minutes
  4. customThe precipitate was collected
  5. washwashed with EtOH (2 mL)
  6. customdried under reduced pressure at 70° C. overnight

出典と根拠

ORDレコード
ord-aa073ff10f4a4991829ed58ac26778ed
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09242973B2

反応ノート

読み込み中…

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