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Diisopropylethylamine → HCID 68616629、化合物

HRID 714456
ノート
印刷プレビュー

反応式

HRID 714456 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([S:8][CH2:9][C:10]2[CH:11]=[C:12]([C:16](O)=[O:17])[CH:13]=[CH:14][CH:15]=2)[C:5]([C:19]#[N:20])=[C:4]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:3]=1[C:27]#[N:28].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH2:53][CH2:54][CH2:55][NH:56][C:57](=[O:63])[O:58][C:59]([CH3:62])([CH3:61])[CH3:60].C(N(CC)C(C)C)(C)C>CN(C=O)C.O1CCCC1.O>[NH2:1][C:2]1[N:7]=[C:6]([S:8][CH2:9][C:10]2[CH:11]=[C:12]([C:16]([NH:53][CH2:54][CH2:55][NH:56][C:57](=[O:63])[O:58][C:59]([CH3:60])([CH3:62])[CH3:61])=[O:17])[CH:13]=[CH:14][CH:15]=2)[C:5]([C:19]#[N:20])=[C:4]([C:21]2[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=2)[C:3]=1[C:27]#[N:28]
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

8

反応物 4

HCID 81531DiisopropylethylamineHCID 187201N-BOC-ethylenediamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 66631614HCID 66631614、化合物

生成物 1

HCID 68616629HCID 68616629、化合物

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 6228Dimethylformamide溶媒
HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

200 mg (0.52 mmol) of 3-{[(6-amino-3,5-dicyano-4-phenylpyridin-2-yl)sulfanyl]methyl}-benzenecarboxylic acid (Example 11) were charged in 5 ml of DMF. The reaction solution was cooled to 0° C. 393.58 mg (1.04 mmol) of HATU were added, and the mixture was then stirred at 0° C. for 20 min. 165.84 mg (1.04 mmol) of tert-butyl (2-aminoethyl)carbamate and 133.78 mg (1.04 mmol) of N,N-diisopropylethylamine were added, and the reaction solution was stirred at RT overnight. Water and tetrahydrofuran were added to the reaction mixture until a clear solution had formed. The solution was purified by preparative HPLC (Chromasil, water/acetonitrile+0.1% trifluoroacetic acid).

後処理

  1. stirringthe reaction solution was stirred at RT overnight
  2. customhad formed
  3. customThe solution was purified by preparative HPLC (Chromasil, water/acetonitrile+0.1% trifluoroacetic acid)

出典と根拠

ORDレコード
ord-5ea8361f48b54957adc9901f54c105f6
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09187428B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート