Trifluoroacetic acid → HCID 25050873, 화합물

HRID 1020250노트

반응식

HRID 1020250 반응식
[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]

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 7519AnisoleHCID 86622751HCID 86622751, 화합물

생성물 1

HCID 25050873HCID 25050873, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-d80f64f82d8142f887ff464e1b22859b
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08716320B2

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