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2,4-Dichloro-1,3,5-triazine → HCID 22028121、化合物

HRID 983423
ノート
印刷プレビュー

反応式

HRID 983423 の反応式
Cl[C:2]1[N:7]=[C:6]([Cl:8])[N:5]=[CH:4][N:3]=1.CCN(C(C)C)C(C)C.[CH3:18][O:19][C:20]1[CH:21]=[C:22]([CH:24]=[C:25]([O:29][CH3:30])[C:26]=1[O:27][CH3:28])[NH2:23]>CN(C=O)C.CCOC(C)=O>[Cl:8][C:6]1[N:5]=[CH:4][N:3]=[C:2]([NH:23][C:22]2[CH:24]=[C:25]([O:29][CH3:30])[C:26]([O:27][CH3:28])=[C:20]([O:19][CH3:18])[CH:21]=2)[N:7]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 178102,4-Dichloro-1,3,5-triazineHCID 322853,4,5-TrimethoxyanilineHCID 81531Diisopropylethylamine

生成物 1

HCID 22028121HCID 22028121、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

2,4-Dichloro-1,3,5-triazine (1.054 g, 7.028 mmol) was dissolved in DMF (5 ml) and cooled to 0° C. To this solution, DIEA (1.225 ml, 7.028 mmol) and 3,4,5-trimethoxyaniline (1.185 g, 6.47 mmol) were added. The reaction mixture was kept at 0° C. for 15 to 30 min and at RT for 2 h. The reaction mixture was diluted with EtOAc and washed with brine. The organic layer was dried over Na2SO4, filtered, and evaporated in vacuo. The residue was added to CH2Cl2 and the resulting white precipitate was filtered and dried under reduced pressure to give (4-chloro-[1,3,5]triazin-2-yl)-(3,4,5-trimethoxy-phenyl)amine: MS m/z=279 [M−Cl+OH2]+. Calc'd for C12H13ClN4O3: 296.

後処理

  1. washwashed with brine
  2. dry with materialThe organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. customevaporated in vacuo
  5. additionThe residue was added to CH2Cl2
  6. filtrationthe resulting white precipitate was filtered
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-997d739a799647c9899f558db2ab8997
出典データセット
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06864255B2

反応ノート

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