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Diisopropylethylamine → HCID 118308243、化合物

HRID 1750518
ノート
印刷プレビュー

反応式

HRID 1750518 の反応式
[NH2:1][C@H:2]1[CH2:6][CH2:5][CH2:4][C@@H:3]1[NH:7][C:8](=[O:14])[O:9][C:10]([CH3:13])([CH3:12])[CH3:11].Cl[C:16]1[CH:21]=[N:20][C:19]([C:22]([F:25])([F:24])[F:23])=[CH:18][N:17]=1.CCN(C(C)C)C(C)C>CS(C)=O>[F:23][C:22]([F:25])([F:24])[C:19]1[N:20]=[CH:21][C:16]([NH:1][C@H:2]2[CH2:6][CH2:5][CH2:4][C@@H:3]2[NH:7][C:8](=[O:14])[O:9][C:10]([CH3:11])([CH3:13])[CH3:12])=[N:17][CH:18]=1
参加物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 17040218(1S,2S)-trans-N-Boc-1,2-cyclopentanediamineHCID 189876452-Chloro-5-(trifluoromethyl)pyrazine

生成物 1

HCID 118308243HCID 118308243、化合物

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A solution of tert-butyl N-[(1S,2S)-2-aminocyclopentyl]carbamate (CAS number 586961-34-4; 1 g, 4.99 mmol), 2-chloro-5-(trifluoromethyl)pyrazine (CAS number 799557-87-2; 1.09 g, 5.99 mmol) and DIPEA (2.62 ml, 14.98 mmol) in DMSO (17 ml) was subjected to microwave irradiation at 140° C. for 1 hour. The reaction was partitioned between ethyl acetate and water, washed with water, brine, dried over magnesium sulfate and concentrated in vacuo. The resulting residue was purified by column chromatography (silica, 0-100% ethyl acetate/petrol) to afford the title compound.

後処理

  1. customirradiation at 140° C. for 1 hour
  2. customThe reaction was partitioned between ethyl acetate and water
  3. washwashed with water, brine
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe resulting residue was purified by column chromatography (silica, 0-100% ethyl acetate/petrol)

出典と根拠

ORDレコード
ord-099b5ba8436b42818a6516957a55482e
出典データセット
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09156829B2

反応ノート

読み込み中…

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