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Sodium Bicarbonate → HCID 178435524、化合物

HRID 384376
ノート
印刷プレビュー

反応式

HRID 384376 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+].[CH2:23]([CH:25]1[C:33]2[C:28](=[CH:29][CH:30]=[C:31]([N:34]3[C:38](=[O:39])[CH2:37][C:36]([CH3:40])=[N:35]3)[CH:32]=2)[CH2:27][CH2:26]1)[CH3:24].C(=O)(O)[O-].[Na+]>Cl.C(O)C>[CH2:23]([CH:25]1[C:33]2[C:28](=[CH:29][CH:30]=[C:31]([N:34]3[C:38](=[O:39])[C:37](=[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:36]([CH3:40])=[N:35]3)[CH:32]=2)[CH2:27][CH2:26]1)[CH3:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 516892Sodium BicarbonateHCID 23668193Sodium NitriteHCID 574837832-(3-Ethyl-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 178435524HCID 178435524、化合物収率 36.4%

試薬・触媒・溶媒 2

HCID 313
Hydrochloric Acid
溶媒
HCID 702Ethanol溶媒

実験手順

3′-Amino-2′-hydroxy-biphenyl-3-carboxylic acid hydrobromide 1f (285 mg, 0.92 mmol) was dissolved in 3.1 mL of hydrochloric acid (1 N) upon cooling by an ice-water bath, followed by dropwise addition of 1.2 mL of aqueous sodium nitrite (70 mg, 1.01 mmol). After the mixture was stirred for 20 minutes, 2-(3-ethyl-indan-5-yl)-5-methyl-2,4-dihydro-pyrazol-3-one 41d (200 mg, 0.83 mmol) was added. The mixture was adjusted to pH 8 with saturated aqueous sodium bicarbonate followed by addition of 2 mL of ethanol. The reaction mixture was warmed up to room temperature overnight. The reaction was monitored by TLC until the disappearance of the starting materials. The mixture was filtered and the filter cake was added to 20 mL of water. The mixture was adjusted to pH 3˜4 with concentrated hydrochloric acid. The mixture was filtered and the filter cake was dried to obtain the title compound 3′-{N′-[1-(3-ethyl-indan-5-yl)-3-methyl-5-oxo-1,5-dihydro-pyrazol-4-ylidene]-hydrazino}-2′-hydroxy-biphenyl-3-carboxylic acid 41 (145 mg, yield 36.4%) as a red solid.

後処理

  1. temperatureupon cooling by an ice-water bath
  2. filtrationThe mixture was filtered
  3. additionthe filter cake was added to 20 mL of water
  4. filtrationThe mixture was filtered
  5. customthe filter cake was dried

出典と根拠

ORDレコード
ord-9306d1c560ad4668afc3926e4a694efd
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