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Ethanolamine → (9H-fluoren-9-yl)methyl N-(2-hydroxyethyl)carbamate

HRID 1449429
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반응식

HRID 1449429 반응식
[NH2:1][CH2:2][CH2:3][OH:4].[CH:5]1[C:17]2[CH:16]([CH2:18][O:19][C:20](Cl)=[O:21])[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9]=2[CH:8]=[CH:7][CH:6]=1.N1C=CC=CC=1>ClCCl>[CH:5]1[C:17]2[CH:16]([CH2:18][O:19][C:20]([NH:1][CH2:2][CH2:3][OH:4])=[O:21])[C:15]3[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=3)[C:9]=2[CH:8]=[CH:7][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 700EthanolamineHCID 1049PyridineHCID 343679-Fluorenylmethyl chloroformate

생성물 1

HCID 2817739(9H-fluoren-9-yl)methyl N-(2-hydroxyethyl)carbamate

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

2-Aminoethanol (1.2 g, 19.7 mmol) in dry dichloromethane (5 ml) was added dropwise to a solution of 9-fluorenylmethylchloroformate (5.0 g, 19.3 mmol) together with pyridine (1.5 g, 19.4 mmol). The mixture was stirred for a total of 1.25 hours then diluted with dichloromethane (50 ml), washed with water (25 ml), a saturated solution of ammonium chloride (25 ml), the organic phase was separated dried over anhydrous magnesium sulphate, filtered and the filtrate evaporated in vacuo to give a white solid. This material was crystallised from dichloromethane to give 2-(9-fluorenylmethoxycarbonyl)aminoethanol.

후처리

  1. washwashed with water (25 ml)
  2. customa saturated solution of ammonium chloride (25 ml), the organic phase was separated
  3. dry with materialdried over anhydrous magnesium sulphate
  4. filtrationfiltered
  5. customthe filtrate evaporated in vacuo
  6. customto give a white solid
  7. customThis material was crystallised from dichloromethane

출처 및 근거

ORD 기록
ord-d62cdf78789247babcad0b29fc24bc37
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05599587

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