Ethyl orthoformate → HCID 67081546、化合物

HRID 2216927ノート

反応式

HRID 2216927 の反応式
[CH3:1][O:2][C:3]([N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[C:9](=[O:16])[CH2:8][C:7]2[CH:17]=[CH:18][CH:19]=[CH:20][C:6]1=2)=[O:4].C(OCC)(OCC)O[CH2:23][CH3:24]>C(O)C.C1(C)C=CC(S(O)(=O)=O)=CC=1>[CH3:1][O:2][C:3]([N:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[C:9]([O:16][CH2:23][CH3:24])=[CH:8][C:7]2[CH:17]=[CH:18][CH:19]=[CH:20][C:6]1=2)=[O:4]

参加物

5

反応物 2

HCID 31214Ethyl orthoformateHCID 1134617110-Oxo-10,11-dihydro-dibenzo[b,f]azepine-5-carboxylic acid methyl ester

生成物 1

HCID 67081546HCID 67081546、化合物収率 97%

試薬・触媒・溶媒 2

HCID 6101p-Toluenesulfonic acid触媒HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

A suspension of 10-oxo-10,11-dihydro-dibenzo[b,f]azepine-5-carboxylic acid methyl ester (15 g, 56 mmol) in ethanol (75 ml) is heated to 60° C. and a catalytic amount of p-toluene sulfonic acid (0.213 g, 1.1 mmol) is added. After addition of triethyl ortho-formate (8.73 g, 58.9 mmol) the solution is stirred at 60–70° C. for 4 hours. During this reaction the product precipitates as white crystals. The mixture is cooled to room temperature, filtered and dried to yield 16.0 g of pure title compound (97%).

後処理

  1. customDuring this reaction the product
  2. customprecipitates as white crystals
  3. temperatureThe mixture is cooled to room temperature
  4. filtrationfiltered
  5. customdried

出典と根拠

ORDレコード
ord-6a325c4262a9402c847f5b7f5eae02c4
出典データセット
uspto-grants-2006_09
特許番号
US07112673B2

反応ノート

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