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2,4-Dichloro-1,3,5-triazine → HCID 22496152、化合物

HRID 983429
ノート
印刷プレビュー

反応式

HRID 983429 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.[NH2:18][C:19]1[CH:20]=[C:21]([CH2:25][C:26]([NH2:28])=[O:27])[CH:22]=[CH:23][CH:24]=1>CN(C=O)C.CCOC(C)=O.O>[Cl:8][C:6]1[N:5]=[CH:4][N:3]=[C:2]([NH:18][C:19]2[CH:20]=[C:21]([CH2:25][C:26]([NH2:28])=[O:27])[CH:22]=[CH:23][CH:24]=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

7

反応物 3

HCID 178102,4-Dichloro-1,3,5-triazineHCID 81531DiisopropylethylamineHCID 1088232-(3-Aminophenyl)acetamide

生成物 1

HCID 22496152HCID 22496152、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒2 回
HCID 8857
Ethyl Acetate
溶媒

反応条件

温度
0 °C

実験手順

2,4-Dichloro-1,3,5-triazine (173.7 mg, 1.158 mmol) was dissolved in DMF (1 ml). To the stirring solution, cooled to 0° C., was added DIEA (202 μl, 1.158 mmol). This solution was added dropwise to a 0° C. mix of DMF (1 ml) and 3-aminophenyl acetamide. The reaction was stirred at 0° C. for min and then at RT for 1 h. The reaction mix was diluted with EtOAc and water. The layers were separated, and the aqueous layer was extracted twice with EtOAc. The combined organic layer was washed 3 times with brine, dried over Na2SO4, and concentrated under reduced pressure, giving 2-[3-(4-chloro-[1,3,5]triazin-2-ylamino)-phenyl]acetamide.

後処理

  1. additionThis solution was added dropwise to a 0° C.
  2. additionThe reaction mix
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted twice with EtOAc
  5. washThe combined organic layer was washed 3 times with brine
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-15a91346add4412180086f5edbb71d2c
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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