Dicyclohexylamine → 3-(1-Adamantyl)-4-methoxyethoxymethoxybenzoyl chloride

HRID 1957694ノート

反応式

HRID 1957694 の反応式
[C:1]12([C:11]3[CH:12]=[C:13]([CH:17]=[CH:18][C:19]=3[O:20][CH2:21][O:22][CH2:23][CH2:24][O:25][CH3:26])[C:14](O)=[O:15])[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.C1(NC2CCCCC2)CCCCC1.S(Cl)([Cl:42])=O>ClCCl>[C:1]12([C:11]3[CH:12]=[C:13]([CH:17]=[CH:18][C:19]=3[O:20][CH2:21][O:22][CH2:23][CH2:24][O:25][CH3:26])[C:14]([Cl:42])=[O:15])[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2

参加物

5

反応物 3

HCID 7582DicyclohexylamineHCID 24386Thionyl ChlorideHCID 153780913-(1-Adamantyl)-4-methoxyethoxymethoxybenzoic acid

生成物 1

HCID 572331023-(1-Adamantyl)-4-methoxyethoxymethoxybenzoyl chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 3 g (8.3 mmol) of 3-(1-adamantyl)-4-methoxyethoxymethoxybenzoic acid in 50 ml of anhydrous dichloromethane was introduced into a round-bottomed flask, 1.7 ml (8.3 mmol) of dicyclohexylamine was added and the mixture was stirred for one hour. 600 μl (8.3 mmol) of thionyl chloride were then added and the mixture was stirred for one hour. It was evaporated to dryness, the residue was taken up in anhydrous ethyl ether, the dicyclohexylamine salt was filtered off and the filtrate was evaporated. 3.3 g (100%) of the crude acid chloride, which was used without further purification for the remainder of the synthesis, were recovered.

後処理

  1. stirringthe mixture was stirred for one hour
  2. customIt was evaporated to dryness
  3. filtrationthe dicyclohexylamine salt was filtered off
  4. customthe filtrate was evaporated
  5. custom3.3 g (100%) of the crude acid chloride, which was used without further purification for the remainder of the synthesis
  6. customwere recovered

出典と根拠

ORDレコード
ord-135e90d9bb8d48199517bcdca299b407
出典データセット
uspto-grants-1998_07
特許番号
US05786379

反応ノート

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