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Sulfuric Acid → HCID 135525454, 화합물

HRID 1684105
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HRID 1684105 반응식
S(=O)(=O)(O)O.[O:6]([CH2:13][C:14]([NH:16][C:17]1[C:22]([C:23](=[O:25])[NH2:24])=[C:21]([O:26][CH3:27])[C:20]([NH:28][C:29](=O)[CH2:30][O:31][C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=2)=[C:19]([C:39](=[O:41])[NH2:40])[C:18]=1[O:42][CH3:43])=O)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C(O)(=O)C>[O:31]([CH2:30][C:29]1[NH:40][C:39](=[O:41])[C:19]2[C:20]([N:28]=1)=[C:21]([O:26][CH3:27])[C:22]1[C:23](=[O:25])[NH:24][C:14]([CH2:13][O:6][C:7]3[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=3)=[N:16][C:17]=1[C:18]=2[O:42][CH3:43])[C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 1118Sulfuric AcidHCID 10098241HCID 10098241, 화합물

생성물 1

HCID 135525454HCID 135525454, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a solution consisting of 40 mL of acetic acid and 4 mL of concentrated sulfuric acid, was added 394 mg (0.753 mmol) of 10. The resulting mixture was refluxed for 4 hours. After allowing the mixture to cool to room temperature, the greyish colored precipitate was collected, washed with acetic acid, and then washed with water to afford pure 14 as a yellow solid: 260 mg (71%) yield; dec pt 290° C.; TLC (ethyl acetate/methanol [9:1]), Rf =0.56; IR (KBr pellet) 2967, 1687, 1630, 1599, 1497, 1463, 1427, 1239, 1206, 1066 cm-1 ; 1H NMR (dimethyl-d6 sulfoxide) δ7.32 (4H, t, J=7.4 Hz, aromatic, no assignments made), 7.08 (4H, d, J=7.8 Hz, aromatic, no assignments made), 6.98 (4H, t, J=7.4 Hz, aromatic, no assignments made), 5.02 (4H, s, methylenes), 3.81 (6H, s, methoxys); mass spectrum (EI mode), m/z 486 (P+). Anal. Calcd for C26H22N4O6 : C, 64.19; H, 4.56; N, 11.52. Found; C, 64.09; H, 4.52; N, 11.31.

후처리

  1. temperatureThe resulting mixture was refluxed for 4 hours
  2. customthe greyish colored precipitate was collected
  3. washwashed with acetic acid
  4. washwashed with water

출처 및 근거

ORD 기록
ord-8a338af350624894b46ee7d7f5794c32
출처 데이터셋
uspto-grants-1997_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05639881

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