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Water → 6-{[5-(4-Methoxyphenyl)-6-phenylfuro[2,3-d]pyrimidin-4-yl]amino}hexanenitrile

HRID 1926874
ノート
印刷プレビュー

反応式

HRID 1926874 の反応式
CCN(C(C)C)C(C)C.[NH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]#[N:17].Cl[C:19]1[C:20]2[C:27]([C:28]3[CH:33]=[CH:32][C:31]([O:34][CH3:35])=[CH:30][CH:29]=3)=[C:26]([C:36]3[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=3)[O:25][C:21]=2[N:22]=[CH:23][N:24]=1.O>CN(C=O)C>[CH3:35][O:34][C:31]1[CH:30]=[CH:29][C:28]([C:27]2[C:20]3[C:19]([NH:17][CH2:16][CH2:15][CH2:14][CH2:13][CH2:12][C:11]#[N:10])=[N:24][CH:23]=[N:22][C:21]=3[O:25][C:26]=2[C:36]2[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=2)=[CH:33][CH:32]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 170796-AminohexanenitrileHCID 81531DiisopropylethylamineHCID 580168154-Chloro-5-(4-methoxyphenyl)-6-phenylfuro[2,3-d]pyrimidine

生成物 1

HCID 580169446-{[5-(4-Methoxyphenyl)-6-phenylfuro[2,3-d]pyrimidin-4-yl]amino}hexanenitrile

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

Add 1.15 g (8.9 mmol) DIEA and 0.67 g (5.9 mmol) 6-aminocapronitrile to 1.0 g (3.0 mmol) 4-chloro-5-(4-methoxyphenyl)-6-phenylfuro[2,3-d]pyrimidine in 10 ml DMF and heat for 2 h to 120° C. After cooling, add water to the mixture and extract three times with ethyl acetate. Wash the organic phase with water, with dilute hydrochloric acid and with saturated sodium chloride solution, dry, and concentrate by evaporation. 1.2 g (98% of theor.) of a yellow oil is obtained, and is used as the raw product in further reactions.

後処理

  1. temperatureheat for 2 h to 120° C
  2. temperatureAfter cooling
  3. extractionextract three times with ethyl acetate
  4. washWash the organic phase with water
  5. dry with materialwith dilute hydrochloric acid and with saturated sodium chloride solution, dry
  6. concentrationconcentrate by evaporation
  7. custom1.2 g (98% of theor.) of a yellow oil is obtained

出典と根拠

ORDレコード
ord-aa30485bbd614833803655a3f8135312
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08183246B2

反応ノート

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