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2-Chloroethanol → 2-Chloroethyl monomethoxytrityl ether

HRID 1709740
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HRID 1709740 반응식
[Cl:1][CH2:2][CH2:3][OH:4].[CH3:5][O:6][C:7]1[CH:26]=[CH:25][CH:24]=[CH:23][C:8]=1[C:9](Cl)([C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1.O>N1C=CC=CC=1>[CH3:5][O:6][C:7]1[CH:26]=[CH:25][CH:24]=[CH:23][C:8]=1[C:9]([O:4][CH2:3][CH2:2][Cl:1])([C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=1)[C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 342-ChloroethanolHCID 962WaterHCID 14429619Methoxytrityl chloride

생성물 1

HCID 230366832-Chloroethyl monomethoxytrityl ether수율 91%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

2-Chloroethanol (4.02 ml, 60 mmol) and monomethoxytrityl chloride (9.2643 g, 30 mmol) were stirred in pyridine (150 ml) at room temperature for 3 hours. Cold water (15 ml) was added to the reaction solution and the mixture was stirred for 30 minutes, and the reaction mixture was extracted with chloroform (500 ml) and washed with water (200 ml ×3 times). The organic layer was dried with anhydrous magnesium sulfate. The magnesium sulfate was removed by filtration and the filtrate was distilled under a reduced pressure. n-Hexane (100 ml) was added to the residue to effect crystallization, and thus 9.6307 g (yield=91%) of 2-chloroethyl monomethoxytrityl ether <1> was obtained.

후처리

  1. extractionthe reaction mixture was extracted with chloroform (500 ml)
  2. washwashed with water (200 ml ×3 times)
  3. dry with materialThe organic layer was dried with anhydrous magnesium sulfate
  4. customThe magnesium sulfate was removed by filtration
  5. distillationthe filtrate was distilled under a reduced pressure
  6. additionn-Hexane (100 ml) was added to the residue
  7. customcrystallization

출처 및 근거

ORD 기록
ord-7cf7b2c7bd0c4c1db6f62d8d860b3297
출처 데이터셋
uspto-grants-1990_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04950745

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