Dicyclohexylamine → HCID 22117430、化合物

HRID 1275626ノート

反応式

HRID 1275626 の反応式
[CH3:1][C:2]1[C:3]([S:16][C:17]2[CH:25]=[CH:24][C:20]([C:21](O)=[O:22])=[CH:19][CH:18]=2)=[CH:4][C:5]2[C:6]([CH3:15])([CH3:14])[CH2:7][CH2:8][C:9]([CH3:13])([CH3:12])[C:10]=2[CH:11]=1.C1(NC2CCCCC2)CCCCC1.S(Cl)([Cl:41])=O>ClCCl>[CH3:1][C:2]1[C:3]([S:16][C:17]2[CH:25]=[CH:24][C:20]([C:21]([Cl:41])=[O:22])=[CH:19][CH:18]=2)=[CH:4][C:5]2[C:6]([CH3:15])([CH3:14])[CH2:7][CH2:8][C:9]([CH3:13])([CH3:12])[C:10]=2[CH:11]=1

参加物

5

反応物 3

HCID 7582DicyclohexylamineHCID 24386Thionyl ChlorideHCID 30259184-[(3,5,5,8,8-Pentamethyl-5,6,7,8-tetrahydronaphthalen-2-yl)sulfanyl]benzoic acid

生成物 1

HCID 22117430HCID 22117430、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A solution of 1.4 g (4 mmol) of 4-(3,5,5,8,8-pentamethyl-5,6,7,8-tetrahydro-2-naphthylthio)benzoic acid in 100 ml of anhydrous dichloromethane was introduced into a round-bottomed flask, 900 μl (4.4 mmol) of dicyclohexylamine were added and the mixture was stirred for one hour. Next, 320 μl (4.4 mmol) of thionyl chloride were added and the mixture was stirred for one hour. The reaction medium was evaporated to dryness, taken up in anhydrous ethyl ether, the dicyclohexylamine salt filtered off and the filtrate evaporated. 1.5 g (100%) of the crude acid chloride was recovered which was used as such in the continuation of the synthesis to follow.

後処理

  1. stirringthe mixture was stirred for one hour
  2. customThe reaction medium was evaporated to dryness
  3. filtrationthe dicyclohexylamine salt filtered off
  4. customthe filtrate evaporated
  5. custom1.5 g (100%) of the crude acid chloride was recovered which
  6. customsuch in the continuation of the synthesis

出典と根拠

ORDレコード
ord-f37de56e665c40b78509ecc73a9a5c87
出典データセット
uspto-grants-2000_12
特許番号
US06162815

反応ノート

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