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Tetrahydrofuran → N-{3-[5-(2-fluoro-4-iodophenylamino)-3-(4-methoxybenzyl)-6,8-dimethyl-2,4,7-trioxo-3,4,6,7-tetrahydro-2H-pyrido[4,3-d]pyrimidin-1-yl]-phenyl}-acetamide

HRID 75677
ノート
印刷プレビュー

反応式

HRID 75677 の反応式
C[O-].[Na+].O1CCCC1.[F:9][C:10]1[CH:15]=[C:14]([I:16])[CH:13]=[CH:12][C:11]=1[N:17]1[C:22]2[N:23]([CH3:40])[C:24](=[O:39])[C:25]([CH3:38])=[C:26]([NH:27][C:28]3[CH:29]=[C:30]([NH:34][C:35](=[O:37])[CH3:36])[CH:31]=[CH:32][CH:33]=3)[C:21]=2[C:20](=[O:41])[N:19]([CH2:42][C:43]2[CH:48]=[CH:47][C:46]([O:49][CH3:50])=[CH:45][CH:44]=2)[C:18]1=[O:51]>CO>[F:9][C:10]1[CH:15]=[C:14]([I:16])[CH:13]=[CH:12][C:11]=1[NH:17][C:22]1[N:23]([CH3:40])[C:24](=[O:39])[C:25]([CH3:38])=[C:26]2[C:21]=1[C:20](=[O:41])[N:19]([CH2:42][C:43]1[CH:48]=[CH:47][C:46]([O:49][CH3:50])=[CH:45][CH:44]=1)[C:18](=[O:51])[N:27]2[C:28]1[CH:29]=[C:30]([NH:34][C:35](=[O:37])[CH3:36])[CH:31]=[CH:32][CH:33]=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 8028TetrahydrofuranHCID 10942334Sodium MethoxideHCID 59717402N-{3-[1-(2-fluoro-4-iodophenyl)-3-(4-methoxybenzyl)-6,8-dimethyl-2,4,7-trioxo-1,2,3,4,7,8-hexahydropyrido[2,3-d]pyrimidin-5-ylamino]-phenyl}-acetamide

生成物 1

HCID 59717341N-{3-[5-(2-fluoro-4-iodophenylamino)-3-(4-methoxybenzyl)-6,8-dimethyl-2,4,7-trioxo-3,4,6,7-tetrahydro-2H-pyrido[4,3-d]pyrimidin-1-yl]-phenyl}-acetamide収率 97.4%

試薬・触媒・溶媒

1
HCID 887Methanol溶媒

実験手順

To a solution (305 mg) of 28% sodium methoxide in methanol were added tetrahydrofuran (4.00 ml) and N-{3-[1-(2-fluoro-4-iodophenyl)-3-(4-methoxybenzyl)-6,8-dimethyl-2,4,7-trioxo-1,2,3,4,7,8-hexahydropyrido[2,3-d]pyrimidin-5-ylamino]-phenyl}-acetamide 87 (1.00 g). The wall was washed with tetrahydrofuran (4.00 ml). The mixture was stirred at room temperature for 1.5 hrs., 2N hydrochloric acid (900 μl) was added, and the mixture was concentrated under reduced pressure. To the residue was added isopropyl alcohol, methanol and water, and after refluxing, the mixture was allowed to cool to room temperature with stirring. The precipitated crystals were collected by filtration, washed with methanol, and dried to give N-{3-[5-(2-fluoro-4-iodophenylamino)-3-(4-methoxybenzyl)-6,8-dimethyl-2,4,7-trioxo-3,4,6,7-tetrahydro-2H-pyrido[4,3-d]pyrimidin-1-yl]-phenyl}-acetamide 88 (974 mg, yield 97.2%) as colorless crystals.

後処理

  1. washThe wall was washed with tetrahydrofuran (4.00 ml)
  2. addition, 2N hydrochloric acid (900 μl) was added
  3. concentrationthe mixture was concentrated under reduced pressure
  4. additionTo the residue was added isopropyl alcohol, methanol and water
  5. temperatureafter refluxing
  6. temperatureto cool to room temperature
  7. stirringwith stirring
  8. filtrationThe precipitated crystals were collected by filtration
  9. washwashed with methanol
  10. customdried

出典と根拠

ORDレコード
ord-9f99bf3669cf493490d623c644a4ed46
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08835443B2

反応ノート

読み込み中…

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