Dicyclohexylamine → HCID 22117430, 화합물

HRID 1275626노트

반응식

HRID 1275626 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 22117430HCID 22117430, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f37de56e665c40b78509ecc73a9a5c87
출처 데이터셋
uspto-grants-2000_12
특허 번호
US06162815

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