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Dimethylformamide → Acetic acid 2-(3-{(R)-(4-carbamimidoylphenylamino)-[5-(1-ethylpropoxycarbonyloxymethoxy)-1-pyrimidin-2-yl-1H-[1,2,4]triazol-3-yl]methyl}-2-fluoro-5-methoxyphenoxy)ethyl ester acetic acid salt

HRID 2089699
ノート
印刷プレビュー

反応式

HRID 2089699 の反応式
[NH2:1][C:2](=[N:49]C(OCC(C)=C)=O)[C:3]1[CH:8]=[CH:7][C:6]([NH:9][C@@H:10]([C:27]2[N:31]=[C:30]([O:32][CH2:33][O:34][C:35]([O:37][CH:38]([CH2:41][CH3:42])[CH2:39][CH3:40])=[O:36])[N:29]([C:43]3[N:48]=[CH:47][CH:46]=[CH:45][N:44]=3)[N:28]=2)[C:11]2[C:12]([F:26])=[C:13]([CH:21]=[C:22]([O:24][CH3:25])[CH:23]=2)[O:14][CH2:15][CH2:16][O:17][C:18](=[O:20])[CH3:19])=[CH:5][CH:4]=1.CN(C=O)C>[Pd].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(O)(=O)C>[C:18]([OH:20])(=[O:17])[CH3:19].[C:2]([C:3]1[CH:4]=[CH:5][C:6]([NH:9][C@@H:10]([C:27]2[N:31]=[C:30]([O:32][CH2:33][O:34][C:35]([O:37][CH:38]([CH2:39][CH3:40])[CH2:41][CH3:42])=[O:36])[N:29]([C:43]3[N:44]=[CH:45][CH:46]=[CH:47][N:48]=3)[N:28]=2)[C:11]2[C:12]([F:26])=[C:13]([CH:21]=[C:22]([O:24][CH3:25])[CH:23]=2)[O:14][CH2:15][CH2:16][O:17][C:18](=[O:20])[CH3:19])=[CH:7][CH:8]=1)(=[NH:1])[NH2:49]
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

5

反応物 2

HCID 6228DimethylformamideHCID 86677416Acetic acid 2-(3-{(R)-(4-{amino[2-methylallyloxycarbonylimino]methyl}phenylamino)-[5-(1-ethylpropoxycarbonyloxymethoxy)-1-pyrimidin-2-yl-1H-[1,2,4]triazol-3-yl]methyl}-2-fluoro-5-methoxyphenoxy)ethyl ester

生成物 1

HCID 86677418Acetic acid 2-(3-{(R)-(4-carbamimidoylphenylamino)-[5-(1-ethylpropoxycarbonyloxymethoxy)-1-pyrimidin-2-yl-1H-[1,2,4]triazol-3-yl]methyl}-2-fluoro-5-methoxyphenoxy)ethyl ester acetic acid salt

試薬・触媒・溶媒 2

HCID 11979704
Tetrakis(triphenylphosphine)palladium
触媒
HCID 176Acetic Acid溶媒

反応条件

温度
45 °C

実験手順

To a mixture of acetic acid 2-(3-{(R)-(4-{amino[2-methylallyloxycarbonylimino]methyl}phenylamino)-[5-(1-ethylpropoxycarbonyloxymethoxy)-1-pyrimidin-2-yl-1H-[1,2,4]triazol-3-yl]methyl}-2-fluoro-5-methoxyphenoxy)ethyl ester (Example 51, 266 mg), DMF (2 mL) and acetic acid (0.196 mL), tetrakis(triphenylphosphine) palladium (0) (20 mg) was added, and the resulting mixture was stirred overnight at an external temperature of 45° C. After cooling the mixture to room temperature, the reaction solution containing the captioned compound was divided into 4 equal lots, and used for the following reactions.

後処理

  1. additionwas added
  2. temperatureAfter cooling the mixture to room temperature
  3. additionthe reaction solution containing the captioned compound

出典と根拠

ORDレコード
ord-81ff6cccbf6a45a8bd5a02aea271b8e8
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08436009B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート