3-Amino-1-propanol → N-(3-hydroxypropyl)-4-({4-[4-(trifluoromethyl)phenyl]pyrimidin-2-yl}amino)benzenesulfonamide

HRID 1715692ノート

反応式

HRID 1715692 の反応式
[F:1][C:2]([F:27])([F:26])[C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][N:12]=[C:11]([NH:15][C:16]3[CH:21]=[CH:20][C:19]([S:22](Cl)(=[O:24])=[O:23])=[CH:18][CH:17]=3)[N:10]=2)=[CH:5][CH:4]=1.[NH2:28][CH2:29][CH2:30][CH2:31][OH:32]>C(OCC)(=O)C>[OH:32][CH2:31][CH2:30][CH2:29][NH:28][S:22]([C:19]1[CH:20]=[CH:21][C:16]([NH:15][C:11]2[N:10]=[C:9]([C:6]3[CH:7]=[CH:8][C:3]([C:2]([F:27])([F:26])[F:1])=[CH:4][CH:5]=3)[CH:14]=[CH:13][N:12]=2)=[CH:17][CH:18]=1)(=[O:24])=[O:23]

参加物

4

反応物 2

HCID 90863-Amino-1-propanolHCID 866042824-({4-[4-(Trifluoromethyl)phenyl]pyrimidin-2-yl}amino)benzenesulfonyl chloride

生成物 1

HCID 68673315N-(3-hydroxypropyl)-4-({4-[4-(trifluoromethyl)phenyl]pyrimidin-2-yl}amino)benzenesulfonamide収率 88.4%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

To a solution of 4-({4-[4-(trifluoromethyl)phenyl]pyrimidin-2-yl}amino)benzenesulfonyl chloride (0.10 g, 0.25 mmol) in 2 ml of ethyl acetate is added 3-amino-1-propanol (0.19 g, 2.5 mmol) with stirring, at 0° C. The mixture is stirred at room temperature for 1 hr and then quenched with water (10 ml). The ethyl acetate is evaporated, the resulting suspension is filtered, and the precipitate is washed with water, and hexanes, and then dried in vacuo to give 0.10 g of a white solid; mp 204-205° C.; HRMS: calcd for C20H19F3N4O3S, 452.1130; found (ESI-FTMS, [M+H]1+), 453.12161.

後処理

  1. stirringThe mixture is stirred at room temperature for 1 hr
  2. customquenched with water (10 ml)
  3. customThe ethyl acetate is evaporated
  4. filtrationthe resulting suspension is filtered
  5. washthe precipitate is washed with water, and hexanes
  6. customdried in vacuo

出典と根拠

ORDレコード
ord-ce82a455118041a1bba8380dca4d4443
出典データセット
uspto-grants-2010_09
特許番号
US07799915B2

反応ノート

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