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

HRID 5884

反応式

HRID 5884 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.Cl.Cl.NC1C2CCN(CC2)C1>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 197853Quinuclidine, 3-amino-, 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-aminoquinuclidine dihydrochloride in 20 ml water containing 7.5 g K2CO3. Stirring is continued overnight. The reaction mixture is then diluted with chloroform, the two layers separated and the chloroform layer washed twice with water, dried over magnesium sulfate, filtered and evaporated to dryness to give 1-amino-2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-(N-1-azabicyclo [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. filtrationfiltered
  7. customevaporated to dryness

出典と根拠

ORDレコード
ord-16679a0222a54903abc287b1b5d2fb96
出典データセット
uspto-grants-1993_09
特許番号
US05246942

関連ノート

読み込み中…