Trifluoroacetic acid → HCID 25050873、化合物

HRID 1020250ノート

反応式

HRID 1020250 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][N:9](CC2C=CC(OC)=CC=2OC)[C:10]([NH:12][C:13]2[S:14][CH:15]=[C:16]([CH2:18][O:19][CH2:20][CH2:21][O:22][CH3:23])[N:17]=2)=[O:11])[S:5][C:6]=1[Br:7].C(O)(C(F)(F)F)=O.C1(OC)C=CC=CC=1>O>[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][NH:9][C:10]([NH:12][C:13]2[S:14][CH:15]=[C:16]([CH2:18][O:19][CH2:20][CH2:21][O:22][CH3:23])[N:17]=2)=[O:11])[S:5][C:6]=1[Br:7]

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 7519AnisoleHCID 86622751HCID 86622751、化合物

生成物 1

HCID 25050873HCID 25050873、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Deprotection: The 1-(4,5-Dibromo-thiophen-2-ylmethyl)-1-(2,4-dimethoxy-benzyl)-3-[4-(2-methoxy-ethoxymethyl)-thiazol-2-yl]-urea was treated with TFA followed by the addition of a drop of anisole and a drop of water. Stirred overnight at ambient temperature. The volatiles were removed in vacuo and the crude material was purified by taking up in MeOH and filtering to remove insolubles. The filtrate was concentrated in vacuo, and the resulting solid titrated with ether to give the title compound. 1H NMR (400 MHz, DMSO): 10.70 (br s, 1H), 7.17 (br m, 1H), 7.00 (s, 1H), 6.88 (s, 1H), 4.42 (d, 2H), 4.37 (s, 2H), 3.55 (m, 2H), 3.45 (m, 2H), 3.24 (s, 3H). MS (ES+): M/Z 484, 486 and 488 (M+1).

後処理

  1. customThe volatiles were removed in vacuo
  2. customthe crude material was purified
  3. filtrationfiltering
  4. customto remove insolubles
  5. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-d80f64f82d8142f887ff464e1b22859b
出典データセット
uspto-grants-2014_05
特許番号
US08716320B2

反応ノート

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