Formic Acid → HCID 178432647、化合物

HRID 2200323ノート

反応式

HRID 2200323 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([C:9](=[NH:12])[NH:10][NH2:11])=[N:6][C:7]=1[CH3:8].[CH:13](O)=O>CO>[Br:1][C:2]1[C:7]([CH3:8])=[N:6][C:5]([C:9]2[NH:12][CH:13]=[N:11][N:10]=2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 284Formic AcidHCID 178432964HCID 178432964、化合物

生成物 1

HCID 178432647HCID 178432647、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
100 °C

実験手順

5-Bromo-6-methylpicolin-imido-hydrazide (1 equiv) and formic acid (15 equiv) were combined and heated to 100° C. for 6 h. The reaction was cooled to room temperature and diluted with methanol. The resulting slurry was partially concentrated under reduced pressure and the resulting mixture was diluted with methanol and partially concentrated under reduced pressure. The resulting solids were collected by filtration, washed with water and dried to provide the desired product, as a solid. MS (ESI) m/z 238.9 [M]+, 240.9 [M+2]+.

後処理

  1. temperatureThe reaction was cooled to room temperature
  2. concentrationThe resulting slurry was partially concentrated under reduced pressure
  3. additionthe resulting mixture was diluted with methanol
  4. concentrationpartially concentrated under reduced pressure
  5. filtrationThe resulting solids were collected by filtration
  6. washwashed with water
  7. customdried

出典と根拠

ORDレコード
ord-91ba00941eff47dd9f320718d2efa8dd
出典データセット
uspto-grants-2016_06
特許番号
US09359364B2

反応ノート

読み込み中…