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Diethanolamine → HCID 13850775, 화합물

HRID 1382205
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HRID 1382205 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10]Cl)([O-:3])=[O:2].[OH:12][CH2:13][CH2:14][NH:15][CH2:16][CH2:17][OH:18].C(N(CC)CC)C>C(Cl)Cl>[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10][N:15]([CH2:16][CH2:17][OH:18])[CH2:14][CH2:13][OH:12])([O-:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8113DiethanolamineHCID 8471TriethylamineHCID 243192-Nitrobenzenesulfenyl chloride

생성물 1

HCID 13850775HCID 13850775, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 379 g (2 mol) of 2-nitrophenylsulphenyl chloride in 2 l of methylene chloride is added to a solution of 210 g (2 mol) of bis(2-hydroxyethyl)amine and 202 g (2 mol) of triethylamine in 3 l of methylene chloride in the course of 90 minutes, the temperature rising from 21° to 34°. The mixture is subsequently stirred at room temperature for 2 hours and is left to stand overnight and the solution is washed six times with 1 l of water each time, dried with sodium sulphate and concentrated in vacuo. The residue is an orange-yellow solid product of melting point 82°-86°, which is sufficiently pure for further reaction. Yield: 499 g.

후처리

  1. customrising from 21° to 34°
  2. waitis left
  3. waitto stand overnight
  4. washthe solution is washed six times with 1 l of water each time
  5. dry with materialdried with sodium sulphate
  6. concentrationconcentrated in vacuo
  7. customis sufficiently pure for further reaction

출처 및 근거

ORD 기록
ord-07e49fdbffe24e31812ec43891508cbe
출처 데이터셋
uspto-grants-1989_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04806539

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