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Hydrochloric Acid → HCID 89651135, 화합물

HRID 2174226
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HRID 2174226 반응식
[CH2:1]([NH:3][C:4](=[O:25])[NH:5][C:6]1[CH:16]=[C:15]([NH:17][C:18]2[CH:19]=[C:20]([CH3:24])[CH:21]=[CH:22][CH:23]=2)[C:9]([C:10]([O:12]CC)=[O:11])=[CH:8][N:7]=1)[CH3:2].Cl>[OH-].[Na+]>[CH2:1]([NH:3][C:4](=[O:25])[NH:5][C:6]1[CH:16]=[C:15]([NH:17][C:18]2[CH:19]=[C:20]([CH3:24])[CH:21]=[CH:22][CH:23]=2)[C:9]([C:10]([OH:12])=[O:11])=[CH:8][N:7]=1)[CH3:2]
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 89650477HCID 89650477, 화합물

생성물 1

HCID 89651135HCID 89651135, 화합물

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

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온도
75 °C

실험 절차

A suspension of compound vii (0.140 g, 0.410 mmol) in aqueous sodium hydroxide solution (2M, 3 mL) was heated to 75° C. for 48 h, cooled to 0° C. and acidified to pH ˜2 using concentrated hydrochloric acid (35%). The resulting colourless precipitate was filtered, washed with water (3 mL) and air dried to give the desired compound viii. (0.116 g, 0.369 mmol, 90%) as a colourless powder, 1H NMR (300 MHz, DMSO-d6): δ 9.98 (1H, br s), 9.17 (1H, br s), 8.58 (1H, s), 7.94 (1H, br t), 7.30 (1H, t, J 7.7), 7.20 (1H, s), 7.12-7.06 (2H, m), 7.01 (1H, d, J 7.7), 3.13 (2H, dq, J 6.7 and 7.7), 1.05 (3H, t, J 7.2); [M+H]+ m/z=315.1.

후처리

  1. temperaturecooled to 0° C.
  2. filtrationThe resulting colourless precipitate was filtered
  3. washwashed with water (3 mL) and air
  4. customdried

출처 및 근거

ORD 기록
ord-96e6beb1a50f470295bde920d19fd7e5
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09060515B2

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