Hydroxylamine → n-Hydroxypyrimidine-5-carboximidamide

HRID 578148노트

반응식

HRID 578148 반응식
[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]

참가 물질

4

반응물 2

HCID 787HydroxylamineHCID 10197646Pyrimidine-5-carbonitrile

생성물 1

HCID 34181140n-Hydroxypyrimidine-5-carboximidamide

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-915e37e6bcc4409e9a30b95a1fe6e99b
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040568B2

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