Trichloroacetonitrile → (4-Bromophenyl)(phenyl)methyl 2,2,2 trichloroethanimidoate

HRID 1180444

反応式

HRID 1180444 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[OH:9])=[CH:4][CH:3]=1.[H-].[Na+].[Cl:18][C:19]([Cl:23])([Cl:22])[C:20]#[N:21]>CCOCC>[Cl:18][C:19]([Cl:23])([Cl:22])[C:20](=[NH:21])[O:9][CH:8]([C:5]1[CH:4]=[CH:3][C:2]([Br:1])=[CH:7][CH:6]=1)[C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1

参加物

5

反応物 3

HCID 11011TrichloroacetonitrileHCID 24758Sodium hydrideHCID 98221p-Bromobenzhydryl alcohol

生成物 1

HCID 69473260(4-Bromophenyl)(phenyl)methyl 2,2,2 trichloroethanimidoate

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
0 °C

実験手順

(4-bromophenyl)(phenyl)methanol from example 67 step 2 (175 g, 0.665 mol) was dissolved in Et2O (700 mL) and sodium hydride (2.66 g of 60% dispension in oil, 0.067 mol, 0.1 eg) was added. Reaction mixture was cooled to 0° C. and trichloroacetonitrile (96 g, 0.665 mol, 1 eg) was added dropwise over 15 min. Reaction mixture was allowed to warm to room temperature and stirred for 1.5 hours. Mixture was evaporated to dryness and solid was stirred in hexane for 18 hours. The solid was filtered to give the product.

後処理

  1. customReaction mixture
  2. customReaction mixture
  3. temperatureto warm to room temperature
  4. customMixture was evaporated to dryness and solid
  5. stirringwas stirred in hexane for 18 hours
  6. filtrationThe solid was filtered
  7. customto give the product

出典と根拠

ORDレコード
ord-d6773aef15e24433a995ccf9c597147b
出典データセット
uspto-grants-2007_10
特許番号
US07279478B2

関連ノート

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