Isethionic Acid → 2-Aminomethyl-4-(1,1-dimethylethyl)-6-iodophenol isethionate-hemihydrate

HRID 437211

반응식

HRID 437211 반응식
[NH2:1][CH2:2][C:3]1[CH:8]=[C:7]([C:9]([CH3:12])([CH3:11])[CH3:10])[CH:6]=[C:5]([I:13])[C:4]=1[OH:14].[S:15]([CH2:19][CH2:20][OH:21])([OH:18])(=[O:17])=[O:16]>CC(O)C.CCOCC>[OH2:14].[S:15]([O:18][C:4]1[C:5]([I:13])=[CH:6][C:7]([C:9]([CH3:10])([CH3:12])[CH3:11])=[CH:8][C:3]=1[CH2:2][NH2:1])([CH2:19][CH2:20][OH:21])(=[O:17])=[O:16].[NH2:1][CH2:2][C:3]1[CH:8]=[C:7]([C:9]([CH3:11])([CH3:10])[CH3:12])[CH:6]=[C:5]([I:13])[C:4]=1[O:14][S:15]([CH2:19][CH2:20][OH:21])(=[O:17])=[O:16]

참가 물질

5

반응물 2

HCID 7866Isethionic AcidHCID 1192862-Aminomethyl-4-t-butyl-6-iodophenol

생성물 1

HCID 1317108192-Aminomethyl-4-(1,1-dimethylethyl)-6-iodophenol isethionate-hemihydrate

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 3776Isopropanol용매

실험 절차

To a freshly-prepared solution of 2-aminomethyl-4-(1,1-dimethylethyl)-6-iodophenol (1.95 g., 6.5 millimole) in 2-propanol (20 ml.) is added 6.5N isethionic acid (1 ml., 6.5 milliequivalents) at room temperature. Upon diluting the resulting solution with ether (100 ml.), a white solid precipitates and is collected to 2.4 g., m.p. 160°-163° C. (dec.). Crystallization (twice) of this solid from 2-propanol-ether (2:5; 70 ml.) affords 2-aminomethyl-4-(1,1-dimethylethyl)-6-iodophenol isethionate-hemihydrate as colorless crystals (1.93 g.), m.p. 166°-167.5° C.(dec.).

후처리

  1. customa white solid precipitates
  2. customis collected to 2.4 g
  3. customCrystallization (twice) of this solid from 2-propanol-ether (2:5; 70 ml.)

출처 및 근거

ORD 기록
ord-06607a1668d349f48d6aad3288aea5d6
출처 데이터셋
uspto-grants-1977_06
특허 번호
US04029816

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