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Ammonium Bicarbonate → HCID 178513575, 화합물

HRID 2247152
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HRID 2247152 반응식
[C:1]1([C:7]2([C:12]3[CH:17]=[CH:16][C:15]([C:18]4[NH:22][C:21]5[CH:23]=[CH:24][C:25]([C:27]([NH2:29])=[O:28])=[CH:26][C:20]=5[N:19]=4)=[CH:14][CH:13]=3)[O:11][CH2:10][CH2:9][O:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl:30]C1C=CC(C2(C3C=CC(C4NC5C=CC(C(O)=O)=CC=5N=4)=CC=3)OCCO2)=CC=1.C(N1C=CN=C1)(N1C=CN=C1)=O.C(=O)(O)[O-].[NH4+].[NH4+].[Cl-]>CN(C=O)C>[Cl:30][C:4]1[CH:3]=[CH:2][C:1]([C:7]2([C:12]3[CH:17]=[CH:16][C:15]([C:18]4[NH:22][C:21]5[CH:23]=[CH:24][C:25]([C:27]([NH2:29])=[O:28])=[CH:26][C:20]=5[N:19]=4)=[CH:14][CH:13]=3)[O:8][CH2:9][CH2:10][O:11]2)=[CH:6][CH:5]=1
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참가 물질

7

반응물 5

HCID 14013Ammonium BicarbonateHCID 25517Ammonium ChlorideHCID 682631,1'-CarbonyldiimidazoleHCID 178513574HCID 178513574, 화합물HCID 178524154HCID 178524154, 화합물

생성물 1

HCID 178513575HCID 178513575, 화합물수율 76%

시약·촉매·용매

1
HCID 6228Dimethylformamide용매

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온도
0 °C

실험 절차

2-[4-(2-Phenyl-[1,3]dioxolan-2-yl)-phenyl]-1H-benzoimidazole-5-carboxylic acid amide. To a solution of 2-{4-[2-(4-chloro-phenyl)-[1,3]dioxolan-2-yl]-phenyl}-1H-benzoimidazole-5-carboxylic acid (135 mg, 0.32 mmol) in anhydrous DMF was added carbonyldiimidazole (118 mg, 0.73 mmol). The reaction mixture was stirred under N2 for 30 min and then cooled to 0° C., and ammonium bicarbonate (140 mg, 1.4 mmol) was added. The resulting mixture was allowed to warm to RT and was stirred for 16 h. The mixture was added dropwise to saturated aqueous NH4Cl. The resulting precipitate was collected by filtration and washed with H2O (100 mL) then hexanes (100 mL). The product was dried under vacuum overnight to give the title compound (1.02 mg, 76%). TLC (silica, 1% methanol saturated with ammonia/9% methanol/CH2Cl2): Rf=0.33. HPLC (Method A): Rt=7.42. MS (ESI+): mass calculated for C23H18ClN3O3, 419.1; m/z found, 420.1 [M+H]+. 1H NMR (400 MHz, CD3OD): δ 8.09 (s, 1H), 8.00 (d, J=8.4 Hz, 2H), 7.75-7.72 (dd, J=8.5, 1.5 Hz, 1H), 7.59 (d, J=8.4 Hz, 2H), 7.56 (br d, J=8.7 Hz, 1H), 7.43 (d, J=8.5 Hz, 2H), 7.27 (d, J=8.6 Hz, 2H), 3.99 (s, 4H).

후처리

  1. temperatureto warm to RT
  2. stirringwas stirred for 16 h
  3. filtrationThe resulting precipitate was collected by filtration
  4. washwashed with H2O (100 mL)
  5. customThe product was dried under vacuum overnight

출처 및 근거

ORD 기록
ord-c51e1f1db9984c1c865b35aaf9150f00
출처 데이터셋
uspto-grants-2010_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07687639B2

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