Methyl nitrite → HCID 86759359, 화합물

HRID 48137

반응식

HRID 48137 반응식
[OH-].[Na+].[C:3]([CH2:5][CH:6]=[CH:7][C:8]1[CH:25]=[CH:24][C:11]([CH2:12][C:13]2[CH:18]=[CH:17][C:16]([CH:19]=[CH:20][CH2:21][C:22]#[N:23])=[CH:15][CH:14]=2)=[CH:10][CH:9]=1)#[N:4].[N:26]([O:28]C)=O.[N:30]([O-])=[O:31].[Na+]>CO>[C:22]([C:21](=[N:26][OH:28])[CH:20]=[CH:19][C:16]1[CH:15]=[CH:14][C:13]([CH2:12][C:11]2[CH:24]=[CH:25][C:8]([CH:7]=[CH:6][C:5](=[N:30][OH:31])[C:3]#[N:4])=[CH:9][CH:10]=2)=[CH:18][CH:17]=1)#[N:23]

참가 물질

6

반응물 4

HCID 12231Methyl nitriteHCID 14798Sodium HydroxideHCID 23668193Sodium NitriteHCID 570915964-{4-[4-(3-Cyano-propenyl)-benzyl]-phenyl}-but-3-enenitrile

생성물 1

HCID 86759359HCID 86759359, 화합물수율 76%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A solution of sodium hydroxide (0.8 g; 0.02 mol) in 30 ml of methanol is added to a suspension of 4-{4-[4-(3-cyano-propenyl)-benzyl]-phenyl}-but-3-enenitrile (3.0 g; 0.01 mol), prepared as described in example 6.2, in 20 ml of methanol. Methyl nitrite, generated from 2.07 g (0.03 mol) of sodium nitrite as described in example 2.2, is bubbled through the suspension at 2° C. for 25 min, and the mixture is then left at room temperature for 48 h. The solvent is then evaporated, the residue is dissolved in 200 ml of water, extracted with toluene (the extract is discarded), and acidified with conc. hydrochloric acid. The beige precipitate is taken up in ethyl acetate, washed neutral with water, dried (MgSO4) and concentrated by evaporation. 2.7 g (76%) of 4-{4-[4-(3-cyano-3-hydroxyimino-propenyl)-benzyl]-phenyl}-2-hydroxyimino-but-3-enenitrile are obtained as a light brown solid, melting point 142-145° C. (dec).

후처리

  1. customprepared
  2. customis bubbled through the suspension at 2° C. for 25 min
  3. customThe solvent is then evaporated
  4. dissolutionthe residue is dissolved in 200 ml of water
  5. extractionextracted with toluene (the extract
  6. washwashed neutral with water
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-696874186176498ab615d634fcfa74ee
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06703182B1

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