2-Chlorobenzaldehyde → HCID 86652007、化合物

HRID 1010541ノート

反応式

HRID 1010541 の反応式
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]

参加物

6

反応物 4

HCID 69962-ChlorobenzaldehydeHCID 24083Sulfuric acid magnesium salt (1:1)HCID 5049666Sodium triacetoxyborohydrideHCID 86652006HCID 86652006、化合物

生成物 1

HCID 86652007HCID 86652007、化合物収率 59%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-ef9794a0c4b7466ea036db344c5f5eaa
出典データセット
uspto-grants-2011_07
特許番号
US07977332B2

反応ノート

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