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Water → 2-Amino-4-chloro-6-(3-methyl-pyridin-2-ylmethoxy)-pyrimidine-5-carbonitrile

HRID 1356140
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HRID 1356140 반응식
[NH2:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([C:9]#[N:10])=[C:4](S(C)=O)[N:3]=1.[CH3:14][C:15]1[C:16]([CH2:21][OH:22])=[N:17][CH:18]=[CH:19][CH:20]=1.C1CCN2C(=NCCC2)CC1.O>COCCOC>[NH2:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([C:9]#[N:10])=[C:4]([O:22][CH2:21][C:16]2[C:15]([CH3:14])=[CH:20][CH:19]=[CH:18][N:17]=2)[N:3]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 1514369(3-Methylpyridin-2-yl)methanolHCID 185072772-Amino-4-chloro-6-methanesulfinyl-pyrimidine-5-carbonitrile

생성물 1

HCID 185072242-Amino-4-chloro-6-(3-methyl-pyridin-2-ylmethoxy)-pyrimidine-5-carbonitrile수율 35%

시약·촉매·용매 1

HCID 8071
1,2-Dimethoxyethane
용매

실험 절차

To a stirred suspension of 50 mg (0.23 mmol) 2-amino-4-chloro-6-methanesulfinyl-pyrimidine-5-carbonitrile in 1 ml DME were added 28 mg (0.23 mmol) 3-methyl-2-pyridinemethanol and 521l (0.35 mmol) DBU and stirring continued for 30 min at room temperature. 5 ml water was then added and the resulting crystals collected by filtration and washed with ether to afford 22 mg (35%) 2-amino-4-chloro-6-(3-methyl-pyridin-2-ylmethoxy)-pyrimidine-5-carbonitrile as a white crystalline solid. ES-MS m/e (%): 278 (M{37Cl}+H+, 35), 276 (M{35Cl}+H+, 100).

후처리

  1. filtrationthe resulting crystals collected by filtration
  2. washwashed with ether

출처 및 근거

ORD 기록
ord-6115d30aee184e96a9ca34ca0df71324
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06586441B2

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