Triethylamine → 1-Amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran

HRID 1032840

反応式

HRID 1032840 の反応式
[NH2:1][C:2]1[C:10]2[CH:9]3[CH2:11][CH2:12][CH2:13][CH2:14][CH:8]3[O:7][C:6]=2[C:5](C(O)=O)=[CH:4][C:3]=1[Cl:18].C(N(CC)CC)C.C(OC(Cl)=O)C.C1(N)C(F)=C(F)C(F)=C(N)C=1F.Cl.Cl>C(Cl)(Cl)Cl.O>[NH2:1][C:2]1[C:10]2[CH:9]3[CH2:11][CH2:12][CH2:13][CH2:14][CH:8]3[O:7][C:6]=2[CH:5]=[CH:4][C:3]=1[Cl:18]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 149026Tetrafluoro-m-phenylenediamine dihydrochlorideHCID 151360481-Amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylic acid

生成物 1

HCID 197944301-Amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6212Chloroform溶媒3 回

実験手順

To a cold solution of 0.3 g 1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylic acid in 40 ml chloroform is added 0.3 g of triethylamine and then 0.2 g ethylchloroformate in 10 ml chloroform. Stirring is continued for 2 hours. This is then added to a cold mixture of 3 g 3-aminoguinuclidine dihydrochloride in 20 ml water containing 7.5 g K2CO3. Stirring is continued overnight. The reaction mxiture is then diluted with chloroform, the two layers separated and the chloroform layer washed twice with water, dried over magnesium sulfate and evaporated to dryness to give 1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-(N-1-azabicylo[2.2.2.]oct-3-yl]carboxamide as an oily product.

後処理

  1. stirringStirring
  2. waitis continued overnight
  3. customthe two layers separated
  4. washthe chloroform layer washed twice with water
  5. dry with materialdried over magnesium sulfate
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-cf8788b6d2254ab1ae2405f32d949f17
出典データセット
uspto-grants-1990_09
特許番号
US04959485

関連ノート

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