Trifluoroacetic acid → HCID 178510395, 화합물

HRID 1043268노트

반응식

HRID 1043268 반응식
[C:1]1([C:7]2[CH:12]=[C:11]([CH:13]3[CH2:18][CH2:17][N:16]([CH:19]4[CH2:24][O:23]C(C)(C)[O:21][CH2:20]4)[CH2:15][CH2:14]3)[CH:10]=[CH:9][C:8]=2[NH:27][C:28]([C:30]2[NH:31][CH:32]=[C:33]([C:35]#[N:36])[N:34]=2)=[O:29])[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]=1.[C:37]([OH:43])([C:39]([F:42])([F:41])[F:40])=[O:38]>C1COCC1.O>[F:40][C:39]([F:42])([F:41])[C:37]([OH:43])=[O:38].[C:1]1([C:7]2[CH:12]=[C:11]([CH:13]3[CH2:18][CH2:17][N:16]([CH:19]([CH2:20][OH:21])[CH2:24][OH:23])[CH2:15][CH2:14]3)[CH:10]=[CH:9][C:8]=2[NH:27][C:28]([C:30]2[NH:31][CH:32]=[C:33]([C:35]#[N:36])[N:34]=2)=[O:29])[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 178431605HCID 178431605, 화합물

생성물 1

HCID 178510395HCID 178510395, 화합물수율 60%

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

To a solution of 4-cyano-1H-imidazole-2-carboxylic acid {2-cyclohex-1-enyl-4-[1-(2,2-dimethyl-[1,3]dioxan-5-yl)-piperidin-4-yl]-phenyl}-amide (22 mg, 0.04 mmol, as prepared in the previous step) in THF—H2O (1 mL, 4:1 v/v) was added TFA (0.4 mL), and the reaction was allowed to stir for 1 h. Removal of the solvent under vacuum afforded 14 mg (60%) of the title compound as an amber foam. 1H-NMR (CD3OD, 400 MHz): δ 1.78-1.90 (m, 4H), 2.03-2.16 (m, 3H), 2.29 (br s, 4H), 2.88-2.96 (m, 1H), 3.37-3.40 (m, 1H), 3.46-3.53 (m, 2H), 3.74-3.78 (m, 3H), 5.83 (s, 1H), 7.13 (d, 1H, J=2.0 Hz), 7.22 (dd, 1H, J=2.0, 8.4 Hz), 8.03 (s, 1H), 8.17 (d, 1H, J=8.4 Hz); Mass spectrum (ESI, m/z): Calcd. for C25H31N5O3, 450.2 (M+H). found 450.2.

후처리

  1. customRemoval of the solvent under vacuum

출처 및 근거

ORD 기록
ord-815e01f699d74ea0ac34948435e7d9c8
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08557847B2

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