Hydrochloric Acid → (2,3-Dihydrobenzo[b][1,4]dioxin-2-yl)methyl 4-methylbenzenesulfonate

HRID 963985

반응식

HRID 963985 반응식
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7](Cl)(=[O:9])=[O:8])=[CH:3][CH:2]=1.[O:12]1[C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[O:15][CH2:14][CH:13]1[CH2:22][OH:23].Cl>N1C=CC=CC=1>[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7]([O:23][CH2:22][CH:13]2[O:12][C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=3[O:15][CH2:14]2)(=[O:9])=[O:8])=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 73974-Toluenesulfonyl chlorideHCID 193141,4-Benzodioxane-2-methanol

생성물 1

HCID 4522296(2,3-Dihydrobenzo[b][1,4]dioxin-2-yl)methyl 4-methylbenzenesulfonate수율 85.4%

시약·촉매·용매 1

HCID 1049Pyridine용매2회

실험 절차

A solution of toluene-4-sulphonyl chloride (60.25 g) in pyridine (75 ml) was added dropwise at 20° C. to a stirred solution of 1-(1,4-benzodioxan-2-yl)methanol (50 g) in pyridine (100 ml) and the mixture was stirred at ambient temperature for 18 hours then poured onto an excess of ice and hydrochloric acid (5M). The resulting solid was collected by filtration, washed well with water and dried in vacuo to give 1,4-benzodioxan-2-ylmethyl toluene-4-sulphonate as an off-white solid (82.3 g), m.p. 75°-78° C.

후처리

  1. filtrationThe resulting solid was collected by filtration
  2. washwashed well with water
  3. customdried in vacuo

출처 및 근거

ORD 기록
ord-453116f7021248a1b98c6a004141c30e
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05767116

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