Triethylamine → Ethyl 3-(hexadecyloxy)-2-[(hexadecylthio)methyl]propanoate

HRID 248166ノート

反応式

HRID 248166 の反応式
[CH2:1]([O:17][CH2:18][C:19](=[CH2:25])[C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16].C(N(CC)CC)C.[CH2:33]([SH:49])[CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH3:48]>C(O)C>[CH2:1]([O:17][CH2:18][CH:19]([CH2:25][S:49][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH2:43][CH2:44][CH2:45][CH2:46][CH2:47][CH3:48])[C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 18015HexadecanethiolHCID 12971817Ethyl 2-[(hexadecyloxy)methyl]-2-propenoate

生成物 1

HCID 19764340Ethyl 3-(hexadecyloxy)-2-[(hexadecylthio)methyl]propanoate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a stirred solution of 20 g of ethyl 2-[(hexadecyloxy)methyl]-2-propenoate in 60 ml of ethyl alcohol containing 10 ml of triethylamine is added 53 ml hexadecylmercaptan. Following stirring for 18 hours, the volatile components are removed and the residue is chromatographed by HPLC on silica gel using 9:1 hexanes:ethyl acetate. Fractions containing product are combined and the solvents evaporated to give 32.9 g of the desired product as a white waxy solid.

後処理

  1. customthe volatile components are removed
  2. customthe residue is chromatographed by HPLC on silica gel using 9:1 hexanes
  3. additionFractions containing product
  4. customthe solvents evaporated

出典と根拠

ORDレコード
ord-1a201f6298ac4d309631ce6847600db1
出典データセット
uspto-grants-1993_05
特許番号
US05208223

反応ノート

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