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Diethylamine → HCID 23332913, 화합물

HRID 224395
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HRID 224395 반응식
[CH2:1]([NH:3][CH2:4][CH3:5])[CH3:2].[Cl:6][C:7]([Cl:27])([Cl:26])[CH:8]1[O:13][CH:12]([C:14]([Cl:17])([Cl:16])[Cl:15])[C:11]2[CH:18]=[C:19]([S:22](Cl)(=[O:24])=[O:23])[CH:20]=[CH:21][C:10]=2[O:9]1>C(O)C>[CH2:1]([N:3]([CH2:4][CH3:5])[S:22]([C:19]1[CH:20]=[CH:21][C:10]2[O:9][CH:8]([C:7]([Cl:6])([Cl:26])[Cl:27])[O:13][CH:12]([C:14]([Cl:17])([Cl:15])[Cl:16])[C:11]=2[CH:18]=1)(=[O:24])=[O:23])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 8021DiethylamineHCID 233329662,4-Bis(trichloromethyl)-2H,4H-1,3-benzodioxine-6-sulfonyl chloride

생성물 1

HCID 23332913HCID 23332913, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Diethylamine (0.8 g.) was added dropwise to a stirred suspension of 2,4-bis(trichloromethyl)benzo[1,3]dioxin-6-sulphonyl chloride (4.7 g.) in absolute ethanol (20 ml.), the mixture was maintained under gentle reflux for 2 hours, and the resulting solution was allowed to cool slowly to give a crystalline product, which was recrystallised from aqueous methanol to give 6-diethylsulphamoyl-2,4-bis(trichloromethyl)benzo[1,3]dioxin, m.p. 125°-126° C.

후처리

  1. temperaturethe mixture was maintained
  2. temperatureunder gentle reflux for 2 hours
  3. temperatureto cool slowly
  4. customto give a crystalline product, which
  5. customwas recrystallised from aqueous methanol

출처 및 근거

ORD 기록
ord-9135a77f0285445f92e484d3083d62fa
출처 데이터셋
uspto-grants-1980_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04232032

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