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

HRID 618501

반응식

HRID 618501 반응식
[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

참가 물질

5

반응물 3

HCID 7582DicyclohexylamineHCID 24386Thionyl ChlorideHCID 216241CD 2665

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-243fee5c3bd549d88bb5bc52367f9057
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05952382

연결된 노트

불러오는 중…