Hydrazine hydrate (1:1) → HCID 57742338、化合物

HRID 655267ノート

反応式

HRID 655267 の反応式
[Br:1][C:2]1[CH:3]=[N:4][C:5]2[C:10]([CH:11]=1)=[CH:9][C:8]([CH2:12][C:13]1O[C:16]([NH2:18])=[N:15][N:14]=1)=[CH:7][CH:6]=2.O.[NH2:20][NH2:21]>O>[Br:1][C:2]1[CH:3]=[N:4][C:5]2[C:10]([CH:11]=1)=[CH:9][C:8]([CH2:12][C:13]1[N:20]([NH2:21])[C:16]([NH2:18])=[N:15][N:14]=1)=[CH:7][CH:6]=2

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 68571396HCID 68571396、化合物

生成物 1

HCID 57742338HCID 57742338、化合物収率 49%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
170 °C

実験手順

A mixture of 5-(3-bromo-quinolin-6-ylmethyl)-[1,3,4]oxadiazol-2-ylamine (3.53 g, 11.6 mmol), hydrazine hydrate (30 mL) and water (15 mL) was heated in a microwave vial at 170° C. and 2 bar of pressure for 1 hour. After cooling the formed solid was collected via filtration and washed with cold methanol and dried to return the title compound as white solid (1.79 g, 5.6 mmol, 49%). 1H NMR (DMSO-d6): δ 4.13 (2H, s), 5.46 (s, 2H), 5.56 (s, 2H), 7.23 (d, 1H), 7.81 (s, 1H), 7.98 (d, 1H), 8.71 (d, 1H); 8.91 (d, 1H); MS (m/z) 319 [M+H+]+.

後処理

  1. temperatureAfter cooling the formed solid
  2. filtrationwas collected via filtration
  3. washwashed with cold methanol
  4. customdried

出典と根拠

ORDレコード
ord-7336576d2b214abb934b7c462e355763
出典データセット
uspto-grants-2011_12
特許番号
US08071581B2

反応ノート

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