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

HRID 1926874
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HRID 1926874 반응식
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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-aa30485bbd614833803655a3f8135312
출처 데이터셋
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08183246B2

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