Acetic Acid → Carbonic acid 5-{(R)-(4-carbamimidoylphenylamino)-[2-fluoro-3-(2-hydroxyethoxy)-5-m ethoxyphenyl]methyl}-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester 2-fluoro-1,1-dimethylethyl ester acetic acid salt

HRID 2089703

反応式

HRID 2089703 の反応式
[F:1][CH2:2][C:3]([O:6][C:7](=[O:53])[O:8][CH2:9][O:10][C:11]1[N:12]([C:47]2[N:52]=[CH:51][CH:50]=[CH:49][N:48]=2)[N:13]=[C:14]([C@H:16]([NH:30][C:31]2[CH:36]=[CH:35][C:34]([C:37]([NH2:46])=[N:38]C(OCC(C)=C)=O)=[CH:33][CH:32]=2)[C:17]2[CH:22]=[C:21]([O:23][CH3:24])[CH:20]=[C:19]([O:25][CH2:26][CH2:27][OH:28])[C:18]=2[F:29])[N:15]=1)([CH3:5])[CH3:4].[C:54]([OH:57])(=[O:56])[CH3:55]>[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.CN(C)C=O>[C:54]([OH:57])(=[O:56])[CH3:55].[F:1][CH2:2][C:3]([O:6][C:7](=[O:53])[O:8][CH2:9][O:10][C:11]1[N:12]([C:47]2[N:48]=[CH:49][CH:50]=[CH:51][N:52]=2)[N:13]=[C:14]([C@H:16]([NH:30][C:31]2[CH:36]=[CH:35][C:34]([C:37](=[NH:38])[NH2:46])=[CH:33][CH:32]=2)[C:17]2[CH:22]=[C:21]([O:23][CH3:24])[CH:20]=[C:19]([O:25][CH2:26][CH2:27][OH:28])[C:18]=2[F:29])[N:15]=1)([CH3:5])[CH3:4]

参加物

5

反応物 2

HCID 176Acetic AcidHCID 86677424Carbonic acid 5-{(R)-(4-{amino[2-methylallyloxycarbonylimino]methyl}phenylamino)-[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]methyl}-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester 2-fluoro-1,1-dimethylethyl ester

生成物 1

HCID 86677422Carbonic acid 5-{(R)-(4-carbamimidoylphenylamino)-[2-fluoro-3-(2-hydroxyethoxy)-5-m ethoxyphenyl]methyl}-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester 2-fluoro-1,1-dimethylethyl ester acetic acid salt

試薬・触媒・溶媒 2

HCID 11979704Tetrakis(triphenylphosphine)palladium触媒HCID 6228Dimethylformamide溶媒

反応条件

温度
45 °C

実験手順

Under nitrogen atmosphere, to a mixture of carbonic acid 5-{(R)-(4-{amino-[2-methylallyloxycarbonylimino]methyl}phenylamino)-[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl]methyl}-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester 2-fluoro-1,1-dimethylethyl ester (Example 56b, 63.5 mg), acetic acid (49 μL) and N,N-dimethylformamide (0.70 ml), tetrakis(triphenylphosphine) palladium (0) (4.9 mg) was added, and the resulting mixture was stirred at 45° C. for 15 hours. After cooling the mixture to room temperature, the reaction solution containing the captioned compound was divided into 3 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-82ccc7894e414b3eb62068cda3a22475
出典データセット
uspto-grants-2013_05
特許番号
US08436009B2

関連ノート

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