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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Potassium borohydride → HCID 23458676, 화합물

HRID 1679947
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HRID 1679947 반응식
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9](=[S:16])[S:10][CH2:11][CH2:12][C:13](=[O:15])[CH3:14])=[N:6][CH:7]=1.[BH4-].[K+]>CO.O.C(Cl)(Cl)Cl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([NH:8][C:9](=[S:16])[S:10][CH2:11][CH2:12][CH:13]([OH:15])[CH3:14])=[N:6][CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 4192641Potassium borohydrideHCID 234582413-Oxobutyl 5-chloropyrid-2-yldithiocarbamate

생성물 1

HCID 23458676HCID 23458676, 화합물수율 62.4%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 6212Chloroform용매

실험 절차

The procedure of Example 3 is followed, but a suspension of 3-oxobutyl 5-chloropyrid-2-yldithiocarbamate (17.5 g) in methanol (220 cc) and a solution of potassium borohydride (3.44 g) in distilled water (55 cc) are used as the starting materials at a maximum of 30° C. The reaction is allowed to proceed for 1 hour at between 20° and 30° C. The resulting product (14.2 g; m.p.=115° C.) is dissolved in chloroform (500 cc). The solution is chromatographed on silica (0.2-0.5 mm) (140 g) contained in a column of diameter 3.4 cm. Elution is carried out with chloroform (1,500 cc), this eluate being discarded, and then with chloroform (4 liters). The eluate which is collected is evaporated to dryness under reduced pressure (20 mm Hg) at 45° C. The chromatographed product (11.4 g) is recrystallised from acetonitrile (85 cc). 3-Hydroxybutyl 5-chloropyrid-2-yldithiocarbamate (11.0 g), which melts at 122° C., is obtained.

후처리

  1. customare used as the starting materials at a maximum of 30° C
  2. customThe solution is chromatographed on silica (0.2-0.5 mm) (140 g)
  3. washElution
  4. customThe eluate which is collected
  5. customis evaporated to dryness under reduced pressure (20 mm Hg) at 45° C
  6. customThe chromatographed product (11.4 g) is recrystallised from acetonitrile (85 cc)

출처 및 근거

ORD 기록
ord-564aa2bdbc084dd891affd16bc731163
출처 데이터셋
uspto-grants-1981_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04271167

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