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Sodium borohydride → HCID 14076215, 화합물

HRID 2210330
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HRID 2210330 반응식
[C:1]([NH:9][C:10]1[S:11][CH:12]=[C:13]([C:15](=[O:18])[CH2:16]Br)[N:14]=1)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:19]([C:24]1[CH:29]=[CH:28][C:27]([CH2:30][CH2:31][NH2:32])=[CH:26][CH:25]=1)([O:21][CH2:22][CH3:23])=[O:20].[BH4-].[Na+]>C(Cl)Cl.CO.NC(N)=O>[C:19]([C:24]1[CH:29]=[CH:28][C:27]([CH2:30][CH2:31][NH:32][CH2:16][CH:15]([OH:18])[C:13]2[N:14]=[C:10]([NH:9][C:1](=[O:8])[C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[S:11][CH:12]=2)=[CH:26][CH:25]=1)([O:21][CH2:22][CH3:23])=[O:20]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 4311764Sodium borohydrideHCID 12945884Ethyl 4-(2-aminoethyl)benzoateHCID 14076214HCID 14076214, 화합물

생성물 1

HCID 14076215HCID 14076215, 화합물

시약·촉매·용매 3

HCID 887Methanol용매HCID 1176Urea용매
HCID 6344
Dichloromethane
용매
2회

실험 절차

9.6 g (0.03 mol) of 2-Benzoylamino-4-bromoacetyl-thiazole are dissolved in 100 ml of methylene chloride and, while stirring at room temperature, added dropwise to a solution of 11.5 g (0.06 mol) of 2-(4-carboethoxyphenyl)ethylamine in 150 ml of methylene chloride. After 1.5 hours, the mixture is cooled to 5° C., diluted with 200 ml of methanol and, for the reduction of the resulting amino-ketone, 3 g of sodium borohydride are added in small portions at 0°-5° C. After 3 hours the solution is evaporated to dryness, ice/water is added, and hydrochloric acid is used to acidify. After 10 minutes the mixture is made alkaline with sodium bicarbonate solution and extracted with methylene chloride. The extract is dried over sodium sulphate, concentrated and purified on a silica gel column using chloroform/methanol =9:1, with the addition of 2% ammonia-saturated ethanol, as eluant. The resulting product is induced to crystallise with petroleum ether.

후처리

  1. temperaturethe mixture is cooled to 5° C.
  2. additionare added in small portions at 0°-5° C
  3. customAfter 3 hours the solution is evaporated to dryness, ice/water
  4. additionis added
  5. waitAfter 10 minutes the mixture is made
  6. extractionalkaline with sodium bicarbonate solution and extracted with methylene chloride
  7. dry with materialThe extract is dried over sodium sulphate
  8. concentrationconcentrated
  9. custompurified on a silica gel column
  10. additionwith the addition of 2% ammonia-saturated ethanol
  11. customto crystallise with petroleum ether

출처 및 근거

ORD 기록
ord-536ddc360f04463ba261fcf1827562fc
출처 데이터셋
uspto-grants-1995_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05457205

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