Ammonium Chloride → HCID 178455675、化合物

HRID 603002ノート

反応式

HRID 603002 の反応式
[C:1]1([CH:7]([N:14]2[CH2:17][CH:16]([CH:18]([C:23]3[CH:24]=[C:25]([CH:28]=[C:29]([F:31])[CH:30]=3)[C:26]#[N:27])[C:19]([F:22])([CH3:21])[CH3:20])[CH2:15]2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N-:32]=[N+:33]=[N-:34].[Na+].[Cl-].[NH4+]>CN(C=O)C>[C:1]1([CH:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:14]2[CH2:15][CH:16]([CH:18]([C:23]3[CH:24]=[C:25]([C:26]4[NH:34][N:33]=[N:32][N:27]=4)[CH:28]=[C:29]([F:31])[CH:30]=3)[C:19]([F:22])([CH3:21])[CH3:20])[CH2:17]2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 113390333-{1-[(Diphenylmethyl)azetidin-3-yl]-2-fluoro-2-methylpropyl}-5-fluorobenzonitrile

生成物 1

HCID 178455675HCID 178455675、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 1.17 g (2.81 mmol) of 3-{1-[(diphenylmethyl)azetidin-3-yl]-2-fluoro-2-methylpropyl}-5-fluorobenzonitrile, 914 mg (14.06 mmol) of sodium azide, and 715 mg (14.05 mmol) of ammonium chloride in 15 mL of DMF was stirred for 16 h. Then it was concentrated to remove solvents. The residue was purified by silica gel chromatography with CH2Cl2/MeOH/NH3 (2M) in MeOH to afford the title compound as a white solid;

後処理

  1. concentrationThen it was concentrated
  2. customto remove solvents
  3. customThe residue was purified by silica gel chromatography with CH2Cl2/MeOH/NH3 (2M) in MeOH

出典と根拠

ORDレコード
ord-1036100b0da14d0592a682ab575adb13
出典データセット
uspto-grants-2011_03
特許番号
US07906652B2

反応ノート

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