Dicyclohexylamine → 4-[7-(1-Adamantyl)-6-methoxyethoxymethoxy-2-naphthyl]benzoic acid chloride

HRID 618501

反応式

HRID 618501 の反応式
[C:1]12([C:11]3[CH:20]=[C:19]4[C:14]([CH:15]=[CH:16][C:17]([C:21]5[CH:29]=[CH:28][C:24]([C:25](O)=[O:26])=[CH:23][CH:22]=5)=[CH:18]4)=[CH:13][C:12]=3[O:30][CH2:31][O:32][CH2:33][CH2:34][O:35][CH3:36])[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:52])=O>ClCCl>[C:1]12([C:11]3[CH:20]=[C:19]4[C:14]([CH:15]=[CH:16][C:17]([C:21]5[CH:29]=[CH:28][C:24]([C:25]([Cl:52])=[O:26])=[CH:23][CH:22]=5)=[CH:18]4)=[CH:13][C:12]=3[O:30][CH2:31][O:32][CH2:33][CH2:34][O:35][CH3:36])[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 216241CD 2665

生成物 1

HCID 1317213724-[7-(1-Adamantyl)-6-methoxyethoxymethoxy-2-naphthyl]benzoic acid chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

10 g (20.6 mmol) of 4-[7-(1-adamantyl)-6-methoxyethoxymethoxy-2-naphthyl]benzoic acid and 100 ml of dichloromethane were introduced into a round-bottomed flask and 4.3 ml (21.6 mmol) of dicyclohexylamine were added dropwise. The reaction mixture was stirred at room temperature for one hour and 2.2 ml (21.6 mmol) of thionyl chloride were added dropwise. The reaction mixture was stirred for one hour and was evaporated to dryness, the residue was taken up in ethyl ether, the dicyclohexylamine salt was filtered off and the filtrate was evaporated. 10.4 g (100%) of the crude acid chloride were collected, which acid chloride was used as is in the synthesis to follow.

後処理

  1. stirringThe reaction mixture was stirred for one hour
  2. customwas evaporated to dryness
  3. filtrationthe dicyclohexylamine salt was filtered off
  4. customthe filtrate was evaporated
  5. custom10.4 g (100%) of the crude acid chloride were collected
  6. customas is in the synthesis

出典と根拠

ORDレコード
ord-243fee5c3bd549d88bb5bc52367f9057
出典データセット
uspto-grants-1999_09
特許番号
US05952382

関連ノート

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