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Sodium Hydroxide → 3-Amino-7-vinylquinoline-2-carboxylic acid

HRID 924385
ノート
印刷プレビュー

反応式

HRID 924385 の反応式
C(OC([NH:11][C:12]1[C:13]([C:23]([O:25]CC)=[O:24])=[N:14][C:15]2[C:20]([CH:21]=1)=[CH:19][CH:18]=[C:17](Br)[CH:16]=2)=O)C1C=CC=CC=1.[O-]P([O-])([O-])=O.[K+].[K+].[K+].[CH3:36][C:37]1(C)C(C)(C)OB(C=C)O1.[OH-].[Na+]>C1(P(C2CCCCC2)C2C=CC=CC=2C2C(C(C)C)=CC(C(C)C)=CC=2C(C)C)CCCCC1.NC1C=CC=CC=1C1C=CC=CC=1[Pd]Cl.O.O1CCOCC1>[NH2:11][C:12]1[C:13]([C:23]([OH:25])=[O:24])=[N:14][C:15]2[C:20]([CH:21]=1)=[CH:19][CH:18]=[C:17]([CH:36]=[CH2:37])[CH:16]=2
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

8

反応物 4

HCID 14798Sodium HydroxideHCID 62657Potassium Phosphate, TribasicHCID 52330122-Ethenyl-4,4,5,5-tetramethyl-1,3,2-dioxaborolaneHCID 86726857Ethyl 3-(((benzyloxy)carbonyl)amino)-7-bromoquinoline-2-carboxylate

生成物 1

HCID 867268673-Amino-7-vinylquinoline-2-carboxylic acid

試薬・触媒・溶媒 3

HCID 178439015
HCID 178439015、化合物
触媒
HCID 962Water溶媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
80 °C

実験手順

Ethyl 3-{[(benzyloxy)carbonyl]amino}-7-bromoquinoline-2-carboxylate (1.50 g, 3.49 mmol), K3PO4 (1.48 g, 6.97 mmol), 1,4-dioxane (45 mL), water (7.5 mL) and 4,4,5,5-tetramethyl-2-vinyl-1,3,2-dioxaborolane (0.80 g, 5.2 mmol) were added to a flask. The reaction mixture was purged with nitrogen for 10 min., then dicyclohexyl(2′,4′,6′-triisopropylbiphenyl-2-yl)phosphine-(2′-aminobiphenyl-2-yl)(chloro)palladium (1:1) (0.18 g, 0.23 mmol) was added. The flask was then sealed and the reaction mixture was heated at 80° C. for 1 h, then allowed to cool to room temperature. After the reaction mixture was allowed to cool, aq. NaOH (2.5 M; 45 mL) was added, the resulting cloudy mixture was then heated at 95° C. for 3 h, and then allowed to cool. The crude product formed as a precipitate, which was collected by vacuum filtration and used in the next step without further purification. LCMS calc. for C12H11N2O2 (M+H)+: m/z=215.2. Found: 215.0.

後処理

  1. customThe reaction mixture was purged with nitrogen for 10 min.
  2. customThe flask was then sealed
  3. temperatureto cool to room temperature
  4. temperatureto cool
  5. temperaturethe resulting cloudy mixture was then heated at 95° C. for 3 h
  6. temperatureto cool

出典と根拠

ORDレコード
ord-319ef15571604013af1824a22eb5121c
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09278950B2

反応ノート

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