1-Butanol → 2-(Bromomethyl)-4-(4-chloro-1-naphthalenyloxymethyl)-2-(2,4-dichlorophenyl)-1,3-dioxolane

HRID 1578438

반응식

HRID 1578438 반응식
[Br:1][CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:6]=1[Cl:12])=[O:4].[Cl:13][C:14]1[C:23]2[C:18](=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:17]([O:24][CH2:25][CH:26]([OH:29])[CH2:27]O)=[CH:16][CH:15]=1.CC1C=CC(S(O)(=O)=O)=CC=1.C(O)CCC>O.C1C=CC=CC=1>[Br:1][CH2:2][C:3]1([C:5]2[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:6]=2[Cl:12])[O:29][CH:26]([CH2:25][O:24][C:17]2[C:18]3[C:23](=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:14]([Cl:13])=[CH:15][CH:16]=2)[CH2:27][O:4]1

참가 물질

7

반응물 4

HCID 2631-ButanolHCID 6101p-Toluenesulfonic acidHCID 758282-Bromo-1-(2,4-dichlorophenyl)ethan-1-oneHCID 203326583-(4-Chloro-1-naphthalenyloxy)-1,2-propanediol

생성물 1

HCID 203326952-(Bromomethyl)-4-(4-chloro-1-naphthalenyloxymethyl)-2-(2,4-dichlorophenyl)-1,3-dioxolane

시약·촉매·용매 2

HCID 241Benzene용매HCID 962Water용매

실험 절차

A mixture of 13.6 parts of 2-bromo-1-(2,4-dichlorophenyl)-1-ethanone, 15.2 parts of 3-(4-chloro-1-naphthalenyloxy)-1,2-propanediol, 3 parts of 4-methylbenzenesulfonic acid, 80 parts of butanol and 180 parts of benzene is stirred and refluxed for 24 hours with water-separator. The reaction mixture is evaporated and the residue is triturated in 2-propanol. The product is filtered off and crystallized from butanol, yielding A + B 2-(bromomethyl)-4-(4-chloro-1-naphthalenyloxymethyl)-2-(2,4-dichlorophenyl)-1,3-dioxolane; mp. 122.7°C.

후처리

  1. customThe reaction mixture is evaporated
  2. customthe residue is triturated in 2-propanol
  3. filtrationThe product is filtered off
  4. customcrystallized from butanol

출처 및 근거

ORD 기록
ord-5a2b3aa0982c42baa028b8a68f72a76f
출처 데이터셋
uspto-grants-1976_02
특허 번호
US03936470

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