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Water → HCID 70540935, 화합물

HRID 1702761
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HRID 1702761 반응식
[CH2:1]([N:3]([C@@H:8]1[CH2:14][CH2:13][CH2:12][C:11]2[CH:15]=[CH:16][CH:17]=[CH:18][C:10]=2[C@H:9]1[OH:19])[C:4](=[O:7])[CH2:5]Cl)[CH3:2].[H-].[Na+].O>CN(C)C=O>[CH2:1]([N:3]1[C:4](=[O:7])[CH2:5][O:19][C@@H:9]2[C:10]3[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=3[CH2:12][CH2:13][CH2:14][C@@H:8]12)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24758Sodium hydride2회HCID 70474738HCID 70474738, 화합물

생성물 1

HCID 70540935HCID 70540935, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

The residue from Step A was dissolved in 50 ml of dimethyl formamide and added dropwise to a solution of 0.7 g (0.0146 m) of a 50% oil dispersion of sodium hydride in 50 ml of dimethyl formamide with stirring. After stirring one hour, excess sodium hydride was decomposed by the addition of water. The mixture was extracted twice with ethyl acetate and the extract was back washed with water, dilute, cold hydrochloric acid and saturated aqueous sodium bicarbonate solution. After drying (Na2SO4) the ethyl acetate solution was concentrated to dryness in vacuo to provide crude product.

후처리

  1. stirringAfter stirring one hour
  2. extractionThe mixture was extracted twice with ethyl acetate
  3. washthe extract was back washed with water
  4. additiondilute
  5. dry with materialAfter drying (Na2SO4) the ethyl acetate solution
  6. concentrationwas concentrated to dryness in vacuo
  7. customto provide crude product

출처 및 근거

ORD 기록
ord-a98cd0a5e5d64ed6b4af0a8e39748adf
출처 데이터셋
uspto-grants-1982_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04349548

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