ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Benzaldehyde → HCID 178478185、化合物

HRID 1486571
ノート
印刷プレビュー

反応式

HRID 1486571 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10]2[N:14]=[C:13]([NH2:15])[NH:12][N:11]=2)[CH:5]=[C:6]([Cl:8])[CH:7]=1.[CH:16](=O)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[BH4-].[Na+]>CO>[CH2:16]([NH:15][C:13]1[NH:12][N:11]=[C:10]([NH:9][C:4]2[CH:5]=[C:6]([Cl:8])[CH:7]=[C:2]([Cl:1])[CH:3]=2)[N:14]=1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 240BenzaldehydeHCID 4311764Sodium borohydrideHCID 727146143-Amino-5-(3,5-dichloroanilino)-s-triazole

生成物 1

HCID 178478185HCID 178478185、化合物収率 98%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
-20 °C

実験手順

A solution of N3-(3,5-dichlorophenyl)-1H-1,2,4-triazole-3,5-diamine Intermediate 2 (70 mg, 287 μmol) and benzaldehyde (121.3 mg, 1.14 mmol) in MeOH (3 ml) was stirred at 45° C. for 2 days to give a suspension, cooled to −20° C. and was filtered to collect the solid. The solid was re-suspended in MeOH (5 ml), NaBH4 (65.1 mg, 1.72 mmol) was added and the reaction was stirred for 1 hour. The solvent was removed, and the reaction mixture was redissolved in EtOAc (5 ml) and washed with water (2×4 ml), dried over MgSO4 and concentrated in vacuo. Crystallization from DCM afforded a white solid as desired product (94 mg, 98% yield). MS +m/z: 334 (M+H)+

後処理

  1. customto give a suspension
  2. filtrationwas filtered
  3. customto collect the solid
  4. customThe solvent was removed
  5. dissolutionthe reaction mixture was redissolved in EtOAc (5 ml)
  6. washwashed with water (2×4 ml)
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated in vacuo
  9. customCrystallization from DCM

出典と根拠

ORDレコード
ord-a662fcda1e11437b833c5403411f73f2
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09428469B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート