Ethyl chloroformate → 5-Ethoxycarbonylamino-4-chloro-2-[2-(2,4-di-tert-amylphenoxy)butanamido]phenol

HRID 1388229ノート

反応式

HRID 1388229 の反応式
[NH2:1][C:2]1[C:3]([Cl:32])=[CH:4][C:5]([NH:9][C:10](=[O:31])[CH:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]([CH2:24][CH3:25])([CH3:23])[CH3:22])=[CH:17][C:16]=2[C:26]([CH2:29][CH3:30])([CH3:28])[CH3:27])[CH2:12][CH3:13])=[C:6]([OH:8])[CH:7]=1.Cl[C:34]([O:36][CH2:37][CH3:38])=[O:35]>C(#N)C>[CH2:37]([O:36][C:34]([NH:1][C:2]1[C:3]([Cl:32])=[CH:4][C:5]([NH:9][C:10](=[O:31])[CH:11]([O:14][C:15]2[CH:20]=[CH:19][C:18]([C:21]([CH2:24][CH3:25])([CH3:23])[CH3:22])=[CH:17][C:16]=2[C:26]([CH2:29][CH3:30])([CH3:28])[CH3:27])[CH2:12][CH3:13])=[C:6]([OH:8])[CH:7]=1)=[O:35])[CH3:38]

参加物

4

反応物 2

HCID 10928Ethyl chloroformateHCID 200361922-{2-(2,4-Di-t-amylphenoxy)butanamido}-4-chloro-5-aminophenol

生成物 1

HCID 204719315-Ethoxycarbonylamino-4-chloro-2-[2-(2,4-di-tert-amylphenoxy)butanamido]phenol

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

42 g of the 5-amino-4-chloro-2-[2-(2,4-di-tert-amylphenoxy)butanamido]phenol obtained in Step (i) above was dispersed in acetonitrile to which 10.4 g of ethyl chloroformate was added dropwise under refluxing. After refluxing for 3 hours, the reaction mixture was cooled to deposite crystals. The crystals were collected by filtration and dried to obtain 41.8 g of the above described compound.

後処理

  1. additionwas added dropwise
  2. temperatureunder refluxing
  3. temperatureAfter refluxing for 3 hours
  4. temperaturethe reaction mixture was cooled to deposite crystals
  5. filtrationThe crystals were collected by filtration
  6. customdried
  7. customto obtain 41.8 g of the

出典と根拠

ORDレコード
ord-d18690cbd9534404bf141d0c25842912
出典データセット
uspto-grants-1984_02
特許番号
US04430423

反応ノート

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