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Phosphate → HCID 23434113, 화합물

HRID 1004178
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HRID 1004178 반응식
[N:1]1[CH:6]=[CH:5][C:4]([C:7]2[S:8][C:9]([C:15]3[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=3)=[C:10]([CH3:14])[C:11]=2[CH:12]=[O:13])=[CH:3][CH:2]=1.[BH4-].[Na+].P([O-])([O-])([O-])=O>CO>[OH:13][CH2:12][C:11]1[C:10]([CH3:14])=[C:9]([C:15]2[CH:20]=[CH:19][N:18]=[CH:17][CH:16]=2)[S:8][C:7]=1[C:4]1[CH:5]=[CH:6][N:1]=[CH:2][CH:3]=1
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참가 물질

5

반응물 3

HCID 1061PhosphateHCID 4311764Sodium borohydrideHCID 121127812,5-Di(4-pyridyl)-4-methylthiophene-3-carbaldehyde

생성물 1

HCID 23434113HCID 23434113, 화합물수율 116.4%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To a stirred solution of 2,5-di(4-pyridyl)-4-methylthiophene-3-carbaldehyde (0.145 g) in methanol (10 mL) was added sodium borohydride (0.11 g) at 0° C. The mixture was stirred at room temperature for 30 minutes. Phosphate buffer was added to the reaction mixture and MeOH was removed by evaporation. The residue was extracted with ethyl acetate (30 mL×2). The combined organic layers were washed with brine, dried over MgSO4, and concentrated in vacuo. The resulting residue was purified by flash chromatography eluting with ethyl acetate-CH2Cl2 --MeOH (1:1:0.04) to give the subtitle compound (0.170 g).

후처리

  1. customwas removed by evaporation
  2. extractionThe residue was extracted with ethyl acetate (30 mL×2)
  3. washThe combined organic layers were washed with brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe resulting residue was purified by flash chromatography
  7. washeluting with ethyl acetate-CH2Cl2

출처 및 근거

ORD 기록
ord-86a255cc51c648599cbc3f47bfdc02b0
출처 데이터셋
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06048880

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