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Phosphate → HCID 20074954, 화합물

HRID 703815
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HRID 703815 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:9]([CH2:15][C:16]([O:18]C)=O)[NH:10][C:11]([NH:13][CH3:14])=[O:12])[CH:6]=[CH:7][CH:8]=1.C[O-].[Na+].P([O-])([O-])([O-])=O>CO>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([N:9]2[CH2:15][C:16](=[O:18])[N:13]([CH3:14])[C:11](=[O:12])[NH:10]2)[CH:6]=[CH:7][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 1061PhosphateHCID 10942334Sodium MethoxideHCID 54355381HCID 54355381, 화합물

생성물 1

HCID 20074954HCID 20074954, 화합물수율 46.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of methyl [1-(3-methoxyphenyl)-2-[(methylamino)carbonyl]hydrazino]acetate (1.6 g) in methanol (20 ml) under nitrogen was added a solution of sodium methoxide (8 ml; from sodium (5.2 g) in methanol (150 ml)). After 1 h the mixture was poured into pH 6 phosphate buffer (100 ml) and partitioned with dichloromethane (3×50 ml). The combined, dried organic extracts were evaporated to give a solid which was purified by FCC eluting with System A (7:3) to give, after trituration with System A (1:1), the title compound (650 mg), m.p. 120°-122°.

후처리

  1. custompartitioned with dichloromethane (3×50 ml)
  2. customdried organic extracts were evaporated
  3. customto give a solid which
  4. customwas purified by FCC
  5. washeluting with System A (7:3)
  6. customto give

출처 및 근거

ORD 기록
ord-e90be0a221cb458cb735744233ea790b
출처 데이터셋
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04985427

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