Triethylamine → ethyl 5-[5-[4-[(acetylimino)aminomethyl]phenoxy]pentyloxy]-2-[N,N-bis(1-methylethyl)carbamoyl]phenoxydimethylacetate

HRID 1683827

反応式

Cl.[NH2:2][N:3]=[CH:4][C:5]1[CH:41]=[CH:40][C:8]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][O:15][C:16]2[CH:17]=[CH:18][C:19]([C:31](=[O:39])[N:32]([CH:36]([CH3:38])[CH3:37])[CH:33]([CH3:35])[CH3:34])=[C:20]([CH:30]=2)[O:21][C:22]([CH3:29])([CH3:28])[C:23]([O:25][CH2:26][CH3:27])=[O:24])=[CH:7][CH:6]=1.[C:42](OC1C=CC=CC=1)(=[O:44])[CH3:43].C(N(CC)CC)C>C(Cl)Cl>[C:42]([N:2]=[N:3][CH2:4][C:5]1[CH:6]=[CH:7][C:8]([O:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][O:15][C:16]2[CH:17]=[CH:18][C:19]([C:31](=[O:39])[N:32]([CH:36]([CH3:38])[CH3:37])[CH:33]([CH3:35])[CH3:34])=[C:20]([CH:30]=2)[O:21][C:22]([CH3:28])([CH3:29])[C:23]([O:25][CH2:26][CH3:27])=[O:24])=[CH:40][CH:41]=1)(=[O:44])[CH3:43]

参加物

実験手順

To a mixture of 0.85 g (1.4 mmol) of ethyl 5-[5-[4-(aminoiminomethyl)phenoxy]pentyloxy]-2-[N,N-bis(1-methylethyl)carbamoyl]phenoxydimethylacetate monohydrochloride in 10 ml of methylene chloride is added 0.39 g (2.8 mmol) of phenyl acetate and 1 ml of triethylamine. The mixture is stirred at room temperature for 2 days and then poured onto a silica gel column and eluted with 80% ethyl acetate/hexane, and then pure ethyl acetate to give ethyl 5-[5-[4-[(acetylimino)aminomethyl]phenoxy]pentyloxy]-2-[N,N-bis(1-methylethyl)carbamoyl]phenoxydimethylacetate as a foam; CHN calculated for C33H47N3O7.0.5H2O:

後処理

additionpoured onto a silica gel column
washeluted with 80% ethyl acetate/hexane

出典と根拠

ORDレコード: ord-f962a3977f914f2e863447cb208bb28d
出典データセット: uspto-grants-1997_06
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US05639768

反応式

参加物

反応物 3

生成物 1

試薬・触媒・溶媒 1

実験手順

後処理

出典と根拠

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