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HCID 23508428、化合物 → HCID 23508443、化合物

HRID 1883692
ノート
印刷プレビュー

反応式

HRID 1883692 の反応式
C([O:8][C:9]1[CH:26]=[CH:25][C:12]([CH2:13][N:14]([C:17]2[CH:24]=[CH:23][C:20]([C:21]#[N:22])=[CH:19][CH:18]=2)[CH2:15][CH3:16])=[CH:11][CH:10]=1)C1C=CC=CC=1.[H][H]>C(OCC)(=O)C>[CH2:15]([N:14]([C:17]1[CH:18]=[CH:19][C:20]([C:21]#[N:22])=[CH:23][CH:24]=1)[CH2:13][C:12]1[CH:11]=[CH:10][C:9]([OH:8])=[CH:26][CH:25]=1)[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 23508428HCID 23508428、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 23508443HCID 23508443、化合物収率 35.5%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

The procedure of Preparation Example 9 was repeated, except that 111 mg of 4-[N-(4-benzyloxybenzyl)-N-ethylamino]benzonitrile was used in place of 4-[N-(4-benzyloxybenzyl)-N-methylsulfonylamino]phenyl methanesulfonate, and 3 ml of ethyl acetate was used in place of dioxane. The resulting mixture was stirred for 4 hours under an atmospheric pressure of hydrogen. The reaction mixture was filtered to remove any insoluble matter, and the solvent was distilled off from the filtrate. The resulting crude product was purified by TLC (using a 1:1 mixture of ethyl acetate and hexane as the developing solvent) to obtain 29 mg of 4-[N-ethyl-N-(4-hydroxybenzyl)amino]benzonitrile.

後処理

  1. customThe procedure of Preparation Example 9
  2. filtrationThe reaction mixture was filtered
  3. customto remove any insoluble matter
  4. distillationthe solvent was distilled off from the filtrate
  5. customThe resulting crude product was purified by TLC (
  6. additiona 1:1 mixture of ethyl acetate and hexane as the developing solvent)

出典と根拠

ORDレコード
ord-d028f53fdb8249b28371d39f9ff2b841
出典データセット
uspto-grants-2004_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06762205B1

反応ノート

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