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 Carbonate → 4-Benzyloxy-1-p-tolyl-isoquinoline-3-carboxylic acid butyl ester

HRID 250458
ノート
印刷プレビュー

反応式

HRID 250458 の反応式
[CH2:1]([O:5][C:6]([C:8]1[N:9]=[C:10](Br)[C:11]2[C:16]([C:17]=1[O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[CH:15][CH:14]=[CH:13][CH:12]=2)=[O:7])[CH2:2][CH2:3][CH3:4].B(O)(O)[C:28]1[CH:29]=[CH:30][C:31]([CH3:34])=[CH:32][CH:33]=1.C([O-])([O-])=O.[Na+].[Na+]>C1COCC1.CCO.O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[CH2:1]([O:5][C:6]([C:8]1[N:9]=[C:10]([C:28]2[CH:33]=[CH:32][C:31]([CH3:34])=[CH:30][CH:29]=2)[C:11]2[C:16]([C:17]=1[O:18][CH2:19][C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1)=[CH:15][CH:14]=[CH:13][CH:12]=2)=[O:7])[CH2:2][CH2:3][CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 3

HCID 10340Sodium CarbonateHCID 79799Tolylboronic acidHCID 860145034-Benzyloxy-1-bromo-isoquinoline-3-carboxylic acid butyl ester

生成物 1

HCID 667127544-Benzyloxy-1-p-tolyl-isoquinoline-3-carboxylic acid butyl ester収率 105.8%

試薬・触媒・溶媒 4

HCID 178418397HCID 178418397、化合物
触媒
HCID 702Ethanol溶媒
HCID 962Water溶媒
HCID 8028Tetrahydrofuran溶媒

実験手順

4-Benzyloxy-1-bromo-isoquinoline-3-carboxylic acid butyl ester (207 mg, 0.5 mmol) and Pd(PPh3)4 (23 mg, 0.02 mmol) were dissolved in THF (3 ml) and the solution was stirred for 10 min before a solution of p-tolylboronic acid (68 mg, 0.5 mmol) in EtOH (0.5 ml) and a solution of Na2CO3 (106 mg, 1 mmol) in water (0.5 ml) were added. The resulting mixture was refluxed with stirring for 4 h. Subsequently, the mixture was concentrated in vacuo. To the residue was added water (2 ml) and the mixture was extracted with EtOAc (10 ml). The organic phase was dried over MgSO4 and evaporated in vacuo to give a yellowish oil (225 mg). Purification by flash column chromatography on silica gel using hexanes:EtOAc=94:6 as the eluent gave the title compound as a colorless oil; MS-(+)-ion: M+1=426.2.

後処理

  1. temperatureThe resulting mixture was refluxed
  2. concentrationSubsequently, the mixture was concentrated in vacuo
  3. additionTo the residue was added water (2 ml)
  4. extractionthe mixture was extracted with EtOAc (10 ml)
  5. dry with materialThe organic phase was dried over MgSO4
  6. customevaporated in vacuo

出典と根拠

ORDレコード
ord-7d780f13eeb849039befe3a570707a91
出典データセット
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07863292B2

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