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Sodium borohydride → HCID 16756661, 화합물

HRID 453094
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HRID 453094 반응식
C([O:3][C:4]([C:6]1[S:10][N:9]=[C:8]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=2)[N:7]=1)=O)C.[BH4-].[Na+]>CO>[Cl:17][C:14]1[CH:13]=[CH:12][C:11]([C:8]2[N:7]=[C:6]([CH2:4][OH:3])[S:10][N:9]=2)=[CH:16][CH:15]=1
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참가 물질

4

반응물 2

HCID 4311764Sodium borohydrideHCID 12351253HCID 12351253, 화합물

생성물 1

HCID 16756661HCID 16756661, 화합물수율 101.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 3-(4-chlorophenyl)-[1,2,4]thiadiazole-5-carboxylic acid ethyl ester (0.20 g, 0.74 mmol) in MeOH (10 ml) was added sodium borohydride (0.048 g, 1.26 mmol) portion wise. The resulting reaction mixture was stirred at room temperature for 2 h. After the completion of the reaction (TLC monitoring), the reaction mass was cooled to 0° C., quenched it with 2 ml of water and concentrated under vacuum. Added water (50 ml) and extracted with ethyl acetate (3×50 ml). The combined organic layer was dried over Na2SO4, filtered and concentrated under vacuum to get the product (0.17 g) that was carried forward to the next step without further purification.

후처리

  1. customThe resulting reaction mixture
  2. customAfter the completion of the reaction (TLC monitoring)
  3. temperaturethe reaction mass was cooled to 0° C.
  4. customquenched it with 2 ml of water
  5. concentrationconcentrated under vacuum
  6. extractionAdded water (50 ml) and extracted with ethyl acetate (3×50 ml)
  7. dry with materialThe combined organic layer was dried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-a88b10e22d734b4db81bc5fdf7bdad68
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08492414B2

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