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Hydrochloric Acid → N-[4-(5,6,7,8-Tetrahydropyrazolo[3,4-d]azepin-2(4H)-yl)phenyl]methanesulfonamide

HRID 1364131
ノート
印刷プレビュー

反応式

HRID 1364131 の反応式
[CH3:1][S:2]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([N:12]2[CH:21]=[C:20]3[C:14]([CH2:15][CH2:16][N:17](C(OC(C)(C)C)=O)[CH2:18][CH2:19]3)=[N:13]2)=[CH:8][CH:7]=1)(=[O:4])=[O:3].Cl>O1CCOCC1.CO>[N:13]1[N:12]([C:9]2[CH:8]=[CH:7][C:6]([NH:5][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:11][CH:10]=2)[CH:21]=[C:20]2[CH2:19][CH2:18][NH:17][CH2:16][CH2:15][C:14]=12
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 2

HCID 313Hydrochloric AcidHCID 669308081,1-Dimethylethyl 2-{4-[(methylsulfonyl)amino]phenyl}-4,5,7,8-tetrahydropyrazolo[3,4-d]azepine-6(2H)-carboxylate

生成物 1

HCID 66930788N-[4-(5,6,7,8-Tetrahydropyrazolo[3,4-d]azepin-2(4H)-yl)phenyl]methanesulfonamide

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒2 回

実験手順

To a solution of 1,1-dimethylethyl 2-{4-[(methylsulfonyl)amino]phenyl}-4,5,7,8-tetrahydropyrazolo[3,4-d]azepine-6(2H)-carboxylate (may be prepared as described in Description 39) (16 mg, 0.039 mmol) in dioxan (1 ml) was added 4M hydrochloric acid in dioxan (2 ml). The resulting mixture was stirred at room temperature, under argon, overnight. The reaction mixture was diluted with methanol and then purified by SCX, eluting with methanol and then 2M ammonia/methanol. The basic fractions were combined and solvent evaporated in vacuo to afford the title compound (D40). MS (ES+) m/e 307 [M+H]+.

後処理

  1. custompurified by SCX
  2. washeluting with methanol
  3. customsolvent evaporated in vacuo

出典と根拠

ORDレコード
ord-c42726a43a1b4ea6989e606bfb2eb298
出典データセット
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07888347B2

反応ノート

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