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

HRID 1180444

반응식

HRID 1180444 반응식
[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

참가 물질

5

반응물 3

HCID 11011TrichloroacetonitrileHCID 24758Sodium hydrideHCID 98221p-Bromobenzhydryl alcohol

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
0 °C

실험 절차

(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.

후처리

  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

출처 및 근거

ORD 기록
ord-d6773aef15e24433a995ccf9c597147b
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07279478B2

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