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Triethylamine → 3-Chloro-benzofuro[3,2-c]isoquinoline-5-ol

HRID 869425
ノート
印刷プレビュー

反応式

HRID 869425 の反応式
COC(=O)[CH:4]([C:6]1[CH:11]=[CH:10][C:9]([Cl:12])=[CH:8][C:7]=1[C:13](OC)=[O:14])Br.[OH:18][C:19]1[CH:26]=[CH:25][CH:24]=[CH:23][C:20]=1[C:21]#[N:22].C(N(CC)CC)C>CC#N>[Cl:12][C:9]1[CH:8]=[C:7]2[C:6]([C:4]3[O:18][C:19]4[CH:26]=[CH:25][CH:24]=[CH:23][C:20]=4[C:21]=3[N:22]=[C:13]2[OH:14])=[CH:11][CH:10]=1
参加物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 8471TriethylamineHCID 119072-HydroxybenzonitrileHCID 867222712-(4-Chloro-2-methoxycarbonyl-phenyl)-2-bromo-acetic acid methyl ester

生成物 1

HCID 1785169623-Chloro-benzofuro[3,2-c]isoquinoline-5-ol収率 56.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 19A (crude, 20.29 mmol) and 2-hydroxy-benzonitrile (20.29 mmol) in MeCN (100 mL) was stirred at room temperature. To the solution was added triethylamine (TEA, 20.44 g, 202.9 mmol) dropwise. After addition completed, the reaction was refluxed for 24 hours, then cooled. The precipitated solids were collected by filtration, washed with a small amount of MeCN, then washed with water several times until there was no TEA salt, dried to give pure product 19B (3.1 g).

後処理

  1. additionAfter addition
  2. temperaturethe reaction was refluxed for 24 hours
  3. temperaturecooled
  4. filtrationThe precipitated solids were collected by filtration
  5. washwashed with a small amount of MeCN
  6. washwashed with water several times until there
  7. customdried

出典と根拠

ORDレコード
ord-e40dfa1c9ea24f92b74a4bff7a070602
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08969373B2

反応ノート

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