Diisopropylethylamine → HCID 86659399、化合物

HRID 1187721ノート

反応式

HRID 1187721 の反応式
Cl[C:2]1[CH:7]=[C:6]([Cl:8])[N:5]=[C:4]([NH:9][C@H:10]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH3:11])[N:3]=1.Cl.[OH:20][CH2:21][C:22]1([OH:28])[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1.C(N(CC)C(C)C)(C)C>C(OCCO)C.C(OCC)(=O)C>[Cl:8][C:6]1[N:5]=[C:4]([NH:9][C@H:10]([C:12]2[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=2)[CH3:11])[N:3]=[C:2]([N:25]2[CH2:26][CH2:27][C:22]([CH2:21][OH:20])([OH:28])[CH2:23][CH2:24]2)[CH:7]=1

参加物

6

反応物 3

HCID 81531DiisopropylethylamineHCID 227444724-(Hydroxymethyl)-4-piperidinol hydrochlorideHCID 86659372(S)-4,6-Dichloro-N-[1-(4-fluorophenyl)ethyl]pyrimidin-2-amine

生成物 1

HCID 86659399HCID 86659399、化合物収率 97.2%

試薬・触媒・溶媒 2

HCID 8076Glycol monoethyl ether溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
135 °C

実験手順

150 mg of (S)-4,6-dichloro-N-[1-(4-fluorophenyl)ethyl]pyrimidine-2-amine and 97 mg of 4-(hydroxymethyl)piperidin-4-ol hydrochloride were dissolved in 3 ml of 2-ethoxyethanol, and 274 μl of N,N-diisopropylethylamine was added thereto, and the mixture was stirred at 135° C. for 20 hours. The reaction solution was air-cooled to room temperature, and then diluted with ethyl acetate. The solution was washed in turn with water and brine and then dried over magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 194 mg of the objective compound as brown oil.

後処理

  1. temperatureThe reaction solution was air-cooled to room temperature
  2. washThe solution was washed in turn with water and brine
  3. dry with materialdried over magnesium sulfate
  4. distillationThe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-4dc904e3b3394660b648d25f4ef9e49f
出典データセット
uspto-grants-2014_03
特許番号
US08673891B2

反応ノート

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