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Citric Acid → HCID 178510428、化合物

HRID 340574
ノート
印刷プレビュー

反応式

HRID 340574 の反応式
C[O:2][C:3](=O)[CH:4]([C:9]1[CH:14]=[CH:13][C:12]([NH:15][C:16]([C:18]2[NH:19][CH:20]=[C:21]([C:23]#[N:24])[N:22]=2)=[O:17])=[C:11]([C:25]2[CH2:30][CH2:29][CH2:28][CH2:27][CH:26]=2)[CH:10]=1)[C:5](OC)=[O:6].[BH4-].[Na+].CO.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>C(O)(C)(C)C.CCOC(C)=O>[C:25]1([C:11]2[CH:10]=[C:9]([CH:4]([CH2:3][OH:2])[CH2:5][OH:6])[CH:14]=[CH:13][C:12]=2[NH:15][C:16]([C:18]2[NH:19][CH:20]=[C:21]([C:23]#[N:24])[N:22]=2)=[O:17])[CH2:30][CH2:29][CH2:28][CH2:27][CH:26]=1
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

7

反応物 4

HCID 311Citric AcidHCID 887MethanolHCID 4311764Sodium borohydrideHCID 178500964HCID 178500964、化合物

生成物 1

HCID 178510428HCID 178510428、化合物収率 61%

試薬・触媒・溶媒 2

HCID 6386tert-Butanol溶媒
HCID 8857
Ethyl Acetate
溶媒

反応条件

温度
80 °C

実験手順

To a mixture of 2-{4-[(4-cyano-1H-imidazole-2-carbonyl)-amino]-3-cyclohex-1-enyl-phenyl}-malonic acid dimethyl ester (as prepared in the previous step, 30.0 mg, 0.0710 mmol) and NaBH4 (13.4 mg, 0.355 mmol) in 1 mL of tert-butyl alcohol (t-BuOH) at 80° C. was added MeOH (50 μL) over 5 min. The resulting mixture was stirred at 80° C. for 16 h under Ar. After cooling to RT, the mixture was treated with 10% aq citric acid to a pH of 7. The mixture was then treated with 30 mL of EtOAc, washed with H2O (5 mL) and brine (10 mL). The organic layer was dried (Na2SO4) and concentrated in vacuo. The residue was purified by flash chromatography on silica gel with 1-5% MeOH-DCM to afford 14.1 mg (61%) of the title compound as a white solid: 1H-NMR (CD3OD; 400 MHz): δ 8.00 (s, 1H), 7.54 (dd, 1H, J=8.2, 2.3 Hz), 7.46 (d, 1H, J=2.3 Hz), 7.27 (d, 1H, J=8.2 Hz), 5.59 (m, 1H), 3.71-3.84 (m, 4H), 3.29 (m, 1H), 2.15-2.29 (m, 4H), 1.67-1.84 (m, 4H). Mass spectrum (ESI, m/z): Calcd. for C20H22N4O3, 367.2 (M+H). found 366.8.

後処理

  1. temperatureAfter cooling to RT
  2. washwashed with H2O (5 mL) and brine (10 mL)
  3. dry with materialThe organic layer was dried (Na2SO4)
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by flash chromatography on silica gel with 1-5% MeOH-DCM

出典と根拠

ORDレコード
ord-3d3fd2f222d544e180399f6f3c9fd59e
出典データセット
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08895584B2

反応ノート

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