6-Nitroveratryl alcohol → 4,5-Dimethoxy-2-nitrobenzyl hexadecanesulfonate

HRID 1111556

반응식

HRID 1111556 반응식
[CH3:1][O:2][C:3]1[C:10]([O:11][CH3:12])=[CH:9][C:6]([CH2:7][OH:8])=[C:5]([N+:13]([O-:15])=[O:14])[CH:4]=1.[CH2:16]([S:32](Cl)(=[O:34])=[O:33])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31]>CC(C)=O.C1(NC2CCCCC2)CCCCC1>[CH2:16]([S:32]([O:8][CH2:7][C:6]1[CH:9]=[C:10]([O:11][CH3:12])[C:3]([O:2][CH3:1])=[CH:4][C:5]=1[N+:13]([O-:15])=[O:14])(=[O:34])=[O:33])[CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][CH2:30][CH3:31]

참가 물질

5

반응물 2

HCID 660976-Nitroveratryl alcoholHCID 969231-Hexadecanesulfonyl chloride

생성물 1

HCID 537926464,5-Dimethoxy-2-nitrobenzyl hexadecanesulfonate

시약·촉매·용매 2

HCID 180Acetone용매HCID 7582Dicyclohexylamine용매

실험 절차

To a solution of 5.33 g (0.025 mol) of 4,5-dimethoxy-2-nitrobenzyl alcohol and 8.15 g (0.025 mol) hexadecanesulfonyl chloride in 100 ml of acetone, dicyclohexylamine (5 ml, slight excess) was added via motor driven syringe over 30 minutes. After the addition was complete, the reaction was stirred an additional 30 minutes. The precipitated dicyclohexylamine hydrochloride was removed by filtration and the acetone filtrate reduced in volume in vacuo until most of the product had precipitated (yield 9.5 g, m.p. 81°-82° C.).

후처리

  1. customover 30 minutes
  2. additionAfter the addition
  3. customThe precipitated dicyclohexylamine hydrochloride was removed by filtration
  4. customhad precipitated (yield 9.5 g, m.p. 81°-82° C.)

출처 및 근거

ORD 기록
ord-0bda839b85f6458e8c089dd31d4efe42
출처 데이터셋
uspto-grants-1990_12
특허 번호
US04980096

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