Hydroxylamine → n-Hydroxypyrimidine-5-carboximidamide

HRID 578148ノート

反応式

HRID 578148 の反応式
[N:1]1[CH:6]=[C:5]([C:7]#[N:8])[CH:4]=[N:3][CH:2]=1.[NH2:9][OH:10]>CO>[OH:10][N:9]=[C:7]([C:5]1[CH:6]=[N:1][CH:2]=[N:3][CH:4]=1)[NH2:8]

参加物

4

反応物 2

HCID 787HydroxylamineHCID 10197646Pyrimidine-5-carbonitrile

生成物 1

HCID 34181140n-Hydroxypyrimidine-5-carboximidamide

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of the product of Example 79B (5.47 g, 52 mmol) and aqueous hydroxylamine (Aldrich, 50%, 2.3 mL, 78 mmol) in methanol (50 mL) was stirred at 65° C. for 1 hour and then concentrated under reduced pressure to remove the volatiles. The residue was triturated with EtOAc (30 mL). The precipitates were collected by filtration and dried to give the titled compound. 1H NMR (300 MHz, DMSO-d6) δ 6.14 (s, 2H), 9.03 (s, 2H), 9.18 (s, 1H), 10.06 (s, 1H) ppm; MS (DCI/NH3) m/z 139 (M+H)+, 156 (M+NH4)+.

後処理

  1. concentrationconcentrated under reduced pressure
  2. customto remove the volatiles
  3. customThe residue was triturated with EtOAc (30 mL)
  4. filtrationThe precipitates were collected by filtration
  5. customdried

出典と根拠

ORDレコード
ord-915e37e6bcc4409e9a30b95a1fe6e99b
出典データセット
uspto-grants-2015_05
特許番号
US09040568B2

反応ノート

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