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

Sodium Bicarbonate → HCID 178433836、化合物

HRID 384411
ノート
印刷プレビュー

反応式

HRID 384411 の反応式
Br.[NH2:2][C:3]1[C:4]([OH:18])=[C:5]([C:9]2[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([OH:17])=[O:16])[CH:10]=2)[CH:6]=[CH:7][CH:8]=1.[N:19]([O-])=O.[Na+].[CH3:23][C:24]1([CH3:40])[CH2:32][C:31]2[C:26](=[CH:27][CH:28]=[C:29]([N:33]3[C:37](=[O:38])[CH2:36][C:35]([CH3:39])=[N:34]3)[CH:30]=2)[CH2:25]1.C(=O)(O)[O-].[Na+]>Cl>[CH3:23][C:24]1([CH3:40])[CH2:32][C:31]2[C:26](=[CH:27][CH:28]=[C:29]([N:33]3[C:37](=[O:38])[C:36](=[N:19][NH:2][C:3]4[C:4]([OH:18])=[C:5]([C:9]5[CH:14]=[CH:13][CH:12]=[C:11]([C:15]([OH:17])=[O:16])[CH:10]=5)[CH:6]=[CH:7][CH:8]=4)[C:35]([CH3:39])=[N:34]3)[CH:30]=2)[CH2:25]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 516892Sodium BicarbonateHCID 23668193Sodium NitriteHCID 574837842-(2,2-Dimethyl-indan-5-yl)-5-methyl-2,4-dihydro-pyrazol-3-oneHCID 574837893'-Amino-2'-hydroxy-biphenyl-3-carboxylic acid hydrobromide

生成物 1

HCID 178433836HCID 178433836、化合物収率 7.6%

試薬・触媒・溶媒 1

HCID 313
Hydrochloric Acid
溶媒

実験手順

3′-Amino-2′-hydroxy-biphenyl-3-carboxylic acid hydrobromide 1f (150 mg, 0.5 mmol) was dissolved in hydrochloric acid (1.7 mL, 1 mol/L) upon cooling by an ice-water bath, followed by dropwise addition of 0.6 mL of aqueous sodium nitrite (38 mg, 0.55 mmol). After the mixture was reacted for 20 minutes, 2-(2,2-dimethyl-indan-5-yl)-5-methyl-2,4-dihydro-pyrazol-3-one 45d (109 mg, 0.45 mmol) was added. The mixture was adjusted to pH 8˜9 with saturated aqueous sodium bicarbonate. Then the generated bubbles were quenched with ethanol. The reaction mixture was reacted overnight at room temperature. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was filtered and the filter cake was added to 15 mL of water. The mixture was adjusted to pH 3˜4 with concentrated hydrochloric acid and filtered. The filter cake was washed with ethyl acetate (1 mL×3) and then dried to obtain the title compound 3′-{N′-[1-(2,2-dimethyl-indan-5-yl)-3-methyl-5-oxo-1,5-dihydro-pyrazol-4-ylidene]-hydrazino}-2′-hydroxy-biphenyl-3-carboxylic acid 56 (16 mg, yield 7.6%) as a yellow solid.

後処理

  1. temperatureupon cooling by an ice-water bath
  2. customAfter the mixture was reacted for 20 minutes
  3. customThen the generated bubbles were quenched with ethanol
  4. customThe reaction mixture was reacted overnight at room temperature
  5. filtrationThe mixture was filtered
  6. additionthe filter cake was added to 15 mL of water
  7. filtrationfiltered
  8. washThe filter cake was washed with ethyl acetate (1 mL×3)
  9. customdried

出典と根拠

ORDレコード
ord-b09b378151744bf9a2ac3af9d15a48a3
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367710B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート