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Water → 1-(4-Chloro-2-formyl-phenoxymethyl)-cyclopropanecarbonitrile

HRID 504528
ノート
印刷プレビュー

反応式

HRID 504528 の反応式
[C:1]([C:3]1([CH2:6]OS(C2C=CC(C)=CC=2)(=O)=O)[CH2:5][CH2:4]1)#[N:2].[Cl:18][C:19]1[CH:20]=[CH:21][C:22]([OH:27])=[C:23]([CH:26]=1)[CH:24]=[O:25].C([O-])([O-])=O.[K+].[K+].O>CN(C=O)C.CCOC(C)=O>[Cl:18][C:19]1[CH:20]=[CH:21][C:22]([O:27][CH2:6][C:3]2([C:1]#[N:2])[CH2:5][CH2:4]2)=[C:23]([CH:24]=[O:25])[CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 124815-Chloro-salicylaldehydeHCID 22028201(1-Cyanocyclopropyl)methyl 4-methylbenzenesulfonate

生成物 1

HCID 577501451-(4-Chloro-2-formyl-phenoxymethyl)-cyclopropanecarbonitrile

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of the crude toluene-4-sulfonic acid 1-cyano-cyclopropylmethyl ester in DMF (30 mL) was added 5-chloro-2-hydroxy-benzaldehyde (5.9 g, 38 mmol) and K2CO3 (10.5 g, 76 mmol) slowly. The reaction mixture was placed in a sealed tube and irradiated by microwave reactor at 75° C. for 30 min. After cooled to room temperature, the mixture was poured into water. The solution was diluted with EtOAc (200 mL), washed with water, dried and concentrated to give the title compound as a black oil (4.76 g). The oil was used for next step reaction directly without further purification.

後処理

  1. customThe reaction mixture was placed in a sealed tube
  2. customirradiated by microwave reactor at 75° C. for 30 min
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-a0235571d0f3488a98e5788f096107ce
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07776875B2

反応ノート

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