Ammonia → HCID 58497086、化合物

HRID 2283937ノート

反応式

HRID 2283937 の反応式
[Cl:1][C:2]1[C:7]([CH2:8][CH3:9])=[C:6](Cl)[N:5]=[CH:4][N:3]=1.[NH3:11]>C(O)CCC>[Cl:1][C:2]1[N:3]=[CH:4][N:5]=[C:6]([NH2:11])[C:7]=1[CH2:8][CH3:9]

参加物

4

反応物 2

HCID 222AmmoniaHCID 218284324,6-Dichloro-5-ethylpyrimidine

生成物 1

HCID 58497086HCID 58497086、化合物収率 55%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
100 °C

実験手順

To a mixture of 4,6-Dichloro-5-ethylpyrimidine (22.5 g, 0.12 mol) in 1-butanol (70 mL) in a 1L glass pressure tube was added aqueous ammonia (26%, 150 mL) at RT. The vessel was sealed and heated to 100° C. for 12 h. The reaction mixture was cooled to RT, the resulted solid was filtered, washed with water (50 mL) and dried under vacuum to afford the titled compound (11.0 g, 55%) as white solid. LCMS: Mass found (M+, 158.0). 1H NMR (400 MHz, CDCl3) 8.02 (s, 1H), 7.10 (bs, 2H), 2.57-2.50 (m, 2H), 1.03-0.99 (m, 3H).

後処理

  1. customThe vessel was sealed
  2. temperatureThe reaction mixture was cooled to RT
  3. filtrationthe resulted solid was filtered
  4. washwashed with water (50 mL)
  5. customdried under vacuum

出典と根拠

ORDレコード
ord-aaad08d38d1f4cea9c598189671b3451
出典データセット
uspto-grants-2015_09
特許番号
US09145392B2

反応ノート

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