Triethylamine → HCID 54050382、化合物

反応式

[OH:1][CH2:2][CH2:3][CH2:4][Si:5]1([CH3:19])[O:12][Si:11]([CH3:14])([CH3:13])[O:10][Si:9]([CH3:16])([CH3:15])[O:8][Si:7]([CH3:18])([CH3:17])[O:6]1.C(N(CC)CC)C.[F:27][C:28]([C:73]([F:76])([F:75])[F:74])([O:32][C:33]([F:72])([F:71])[C:34]([F:70])([C:66]([F:69])([F:68])[F:67])[O:35][C:36]([F:65])([F:64])[C:37]([F:63])([C:59]([F:62])([F:61])[F:60])[O:38][C:39]([F:58])([F:57])[C:40]([F:56])([C:52]([F:55])([F:54])[F:53])[O:41][C:42]([F:51])([F:50])[C:43]([F:49])([F:48])[C:44]([F:47])([F:46])[F:45])[C:29](F)=[O:30]>>[F:27][C:28]([C:73]([F:74])([F:75])[F:76])([O:32][C:33]([F:71])([F:72])[C:34]([F:70])([C:66]([F:67])([F:68])[F:69])[O:35][C:36]([F:64])([F:65])[C:37]([F:63])([C:59]([F:62])([F:61])[F:60])[O:38][C:39]([F:57])([F:58])[C:40]([F:56])([C:52]([F:55])([F:54])[F:53])[O:41][C:42]([F:51])([F:50])[C:43]([F:49])([F:48])[C:44]([F:47])([F:46])[F:45])[C:29]([O:1][CH2:2][CH2:3][CH2:4][Si:5]1([CH3:19])[O:12][Si:11]([CH3:14])([CH3:13])[O:10][Si:9]([CH3:16])([CH3:15])[O:8][Si:7]([CH3:18])([CH3:17])[O:6]1)=[O:30]

参加物

反応物 3

HCID 8471Triethylamine

HCID 118188Perfluoro-2,5,8,11-tetramethyl-3,6,9,12-tetraoxapentadecanoyl fluoride

HCID 22677161HCID 22677161、化合物

生成物 1

HCID 54050382HCID 54050382、化合物収率 71.8%

実験手順

A 50 mL round bottom flask equipped with a magnetic stirring bar and an addition funnel was charged with 6.2 g of 98% (3-hydroxypropyl)heptamethylcyclotetrasiloxane (18 mmoles) and 1.8 g of triethylamine (18 mmoles). The mixture was stirred and 15.0 g of 95% perfluoro-2,5,8,11-tetramethyl-3,6,9,12-tetraoxapentadecanoyl fluoride (17 mmoles) was added dropwise. After complete addition of the acid fluoride a gas chromatographic analysis indicated that essentially all of the acid fluoride and most of the cyclosiloxane were consumed with predominately the formation of one product. A 25 mL portion of dilute hydrochloric acid was added to the flask and the two phase mixture was transferred into a separatory funnel and the aqueous layer was separated from the siloxane layer. The siloxane layer was washed with two 25 mL portions of water and the siloxane layer was transferred into a 50 mL round bottom flask and distilled at 118°-28° C. and 0.05 mmHg to yield a fraction of 14.0 g (71% yield) of 99% [3-(perfluoro-2,5,8,11-tetramethyl-3,6,9,12-tetraoxapentadecan-oyl)oxypropyl]heptamethylcyclotetrasiloxane (12.2 mmoles), which corresponds to formula (I) wherein m is 1, n is 3, X is OC(O), and RF is given by formula (II) wherein p is 4, or more specifically as shown in formula (VII) wherein p=4. The product was analyzed by spectroscopy with the following results: