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Acetic Acid → HCID 20562339, 화합물

HRID 848543
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HRID 848543 반응식
[CH2:1]([O:8][C:9](=[O:40])[NH:10][CH2:11][C:12](=[O:39])[NH:13][CH2:14][C:15]1[CH:20]=[CH:19][C:18]([NH:21][C:22]([NH:24][CH2:25][CH2:26][O:27]C(=O)C)=[O:23])=[CH:17][C:16]=1[CH2:31][C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=1[F:38])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C[O-].[Na+].C(O)(=[O:46])C>CO>[CH2:1]([O:8][C:9](=[O:40])[NH:10][CH2:11][C:12](=[O:39])[NH:13][CH2:14][C:15]1[CH:20]=[CH:19][C:18]([NH:21][C:22]([NH:24][CH2:25][CH2:26][OH:27])=[O:23])=[CH:17][C:16]=1[C:31](=[O:46])[C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=1[F:38])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 10942334Sodium MethoxideHCID 20565342HCID 20565342, 화합물

생성물 1

HCID 20562339HCID 20562339, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

250 mg of benzyl{[[2-(o-fluorobenzyl)-4-[3-(2-acetoxyethyl)ureido]phenyl]methylcarbamoyl]methyl}carbamate dissolved in 10 ml of absolute methanol are treated with 50 mg of sodium methylate, stirred at room temperature for 1 hour and buffered with a small amount of acetic acid. The mixture is poured on to ice/10% sodium bicarbonate and extracted with methylene chloride. The organic solution is dried over sodium sulphate, filtered and concentrated. After crystallisation from ether/ethanol, there is obtained benzyl{[[2-(o-fluorobenzoyl)-4-[3-(2-hydroxyethyl)ureido]phenyl]methylcarbamoyl]methyl}carbamate which melts at 117°-120° C.

후처리

  1. extractionextracted with methylene chloride
  2. dry with materialThe organic solution is dried over sodium sulphate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customAfter crystallisation from ether/ethanol

출처 및 근거

ORD 기록
ord-a5292e74e8924b0095415984d4f97388
출처 데이터셋
uspto-grants-1981_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04296031

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