2-Chlorobenzaldehyde → HCID 86652007, 화합물

HRID 1010541노트

반응식

HRID 1010541 반응식
ClC1N=CC(C[NH:9][CH2:10][CH2:11][N:12]2[CH2:16][CH2:15][NH:14][C:13]2=[CH:17][N+:18]([O-:20])=[O:19])=CC=1.[Cl:21][C:22]1[CH:29]=[CH:28][CH:27]=[CH:26][C:23]=1[CH:24]=O.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].S([O-])([O-])(=O)=O.[Mg+2]>ClCCCl>[Cl:21][C:22]1[CH:29]=[CH:28][CH:27]=[CH:26][C:23]=1[CH2:24][NH:9][CH2:10][CH2:11][N:12]1[CH2:16][CH2:15][NH:14][C:13]1=[CH:17][N+:18]([O-:20])=[O:19]

참가 물질

6

반응물 4

HCID 69962-ChlorobenzaldehydeHCID 24083Sulfuric acid magnesium salt (1:1)HCID 5049666Sodium triacetoxyborohydrideHCID 86652006HCID 86652006, 화합물

생성물 1

HCID 86652007HCID 86652007, 화합물수율 59%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

With stirring and cooling in an ice-water bath (0° C.) 0.12 grams (0.0004 mole) of [(6-chloro(3-pyridyl))methyl]{2-[2-(nitromethylene)imidazolidinyl]ethyl]amine, 0.06 gram (0.0004 mole) of 2-chlorobenzaldehyde, 0.13 gram (0.0006 mole) of sodium triacetoxyborohydride and 0.10 gram (0.0008 mole) of magnesium sulfate in about 20 mL of 1,2-dichloroethane were combined. Upon completion of addition, the cooling bath was removed and the reaction mixture was allowed to warm to ambient temperature as it stirred during an 18 hour period. After this time the reaction was quenched by the addition of five mL of water, then the reaction mixture was neutralized to pH of 8-9. The reaction mixture was then extracted with two 50 mL portions of methylene chloride. The combined extracts were dried with sodium sulfate, filtered and concentrated under reduced pressure, yielding 0.07 gram of Compound 501. The

후처리

  1. additionUpon completion of addition
  2. customthe cooling bath was removed
  3. stirringstirred during an 18 hour period
  4. customAfter this time the reaction was quenched by the addition of five mL of water
  5. extractionThe reaction mixture was then extracted with two 50 mL portions of methylene chloride
  6. dry with materialThe combined extracts were dried with sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-ef9794a0c4b7466ea036db344c5f5eaa
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07977332B2

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