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Diisopropylethylamine → 4-[2-Methoxy-1-(3-trifluoromethyl-phenyl)-ethyl]-piperazine-1-carboxylic acid (7-methoxy-thiazolo[5,4-d]pyrimidin-2-yl)-amide

HRID 550845
ノート
印刷プレビュー

反応式

HRID 550845 の反応式
FC(F)(F)C(O)=O.[CH3:8][O:9][CH2:10][CH:11]([N:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1)[C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:21])([F:20])[F:19])[CH:13]=1.C(N(C(C)C)CC)(C)C.C1([O:43][C:44](=O)[NH:45][C:46]2[S:47][C:48]3[N:49]=[CH:50][N:51]=[C:52]([O:55][CH3:56])[C:53]=3[N:54]=2)C=CC=CC=1>C(#N)C>[CH3:56][O:55][C:52]1[C:53]2[N:54]=[C:46]([NH:45][C:44]([N:25]3[CH2:26][CH2:27][N:22]([CH:11]([C:12]4[CH:17]=[CH:16][CH:15]=[C:14]([C:18]([F:20])([F:21])[F:19])[CH:13]=4)[CH2:10][O:9][CH3:8])[CH2:23][CH2:24]3)=[O:43])[S:47][C:48]=2[N:49]=[CH:50][N:51]=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

5

反応物 3

HCID 81531DiisopropylethylamineHCID 59011944(7-Methoxy-thiazolo[5,4-d]pyrimidin-2-yl)-carbamic acid phenyl esterHCID 866165091-[2-Methoxy-1-(3-trifluoromethyl-phenyl)-ethyl]-piperazine trifluoroacetate

生成物 1

HCID 248306114-[2-Methoxy-1-(3-trifluoromethyl-phenyl)-ethyl]-piperazine-1-carboxylic acid (7-methoxy-thiazolo[5,4-d]pyrimidin-2-yl)-amide収率 41%

試薬・触媒・溶媒 1

HCID 6342
Acetonitrile
溶媒

反応条件

温度
70 °C

実験手順

A mixture of 1-[2-Methoxy-1-(3-trifluoromethyl-phenyl)-ethyl]-piperazine trifluoroacetate (160 mg, 0.40 mmol) and diisopropylethylamine (0.35 mL, 2.0 mmole) in acetonitrile (10 mL) was heated at 70° C. for ten minutes. After cooling to room temperature, (7-methoxy-thiazolo[5,4-d]pyrimidin-2-yl)-carbamic acid phenyl ester (120 mg, 0.40 mmol) was added to the above solution. The mixture was stirred at reflux for three hours. LCMS analysis indicated complete consumption of starting material. The reaction was concentrated and the crude was purified using reversed phase HPLC to give 4-[2-Methoxy-1-(3-trifluoromethyl-phenyl)-ethyl]-piperazine-1-carboxylic acid (7-methoxy-thiazolo[5,4-d]pyrimidin-2-yl)-amide (81 mg, 41% yield) as a white powder. LRMS for C21H23F3N6O3S (M+H)+ at m/z=497. The NMR spectrum obtained on the sample is compatible with its structure.

後処理

  1. temperatureAfter cooling to room temperature
  2. temperatureat reflux for three hours
  3. customconsumption of starting material
  4. concentrationThe reaction was concentrated
  5. customthe crude was purified

出典と根拠

ORDレコード
ord-bf4f7b464e46492482aac50877825e9d
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07947692B2

反応ノート

読み込み中…

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