Carbon Dioxide → HCID 58493981、化合物

HRID 2360480ノート

反応式

HRID 2360480 の反応式
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][C:9]=2[CH2:11][OH:12])[CH:4]=[CH:3]1.C([Li])CCC.[C:18](=[O:20])=[O:19].O>C(OCC)C.CCCCCC>[OH:12][CH2:11][C:9]1[CH:8]=[CH:7][CH:6]=[C:5]2[C:10]=1[N:2]([CH3:1])[C:3]([C:18]([OH:20])=[O:19])=[CH:4]2

参加物

7

反応物 4

HCID 280Carbon Dioxide2 回HCID 962WaterHCID 24229741(1-Methyl-1H-indol-7-yl)methanolHCID 178418339Butyllithium

生成物 1

HCID 58493981HCID 58493981、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 8058Hexane溶媒

実験手順

Under argon a solution of 4 g (1-methyl-1H-indol-7-yl)-methanol in 80 ml diethyl ether is added dropwise to 76 ml of a 1.6 M solution of n-butyllithium in hexane at 0° C., while the temperature does not exceed 35° C. Then the mixture is stirred for another 12 hours at ambient temperature and the solution thus obtained is poured onto 30 g of crushed dry ice in 100 ml diethyl ether. The mixture is stirred until all the dry ice has dissolved and the reaction is then stopped by the addition of 40 ml of water. The phases are separated and the organic phase is extracted twice with 20 ml of water. The combined aqueous phases are suction filtered and the filtrate is adjusted to pH 2 with concentrated hydrochloric acid. The solid precipitated is suction filtered and dried in vacuo.

後処理

  1. customdoes not exceed 35° C
  2. customthe solution thus obtained
  3. dissolutionhas dissolved
  4. customThe phases are separated
  5. extractionthe organic phase is extracted twice with 20 ml of water
  6. filtrationfiltered
  7. customThe solid precipitated
  8. filtrationfiltered
  9. customdried in vacuo

出典と根拠

ORDレコード
ord-a5ee6624cb604bbf90ad9fa78ba67e81
出典データセット
uspto-grants-2014_04
特許番号
US08686022B2

反応ノート

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