Pentachlorophenol → HCID 131710245、化合物

HRID 1076838ノート

反応式

HRID 1076838 の反応式
[CH3:1][O:2][C@H:3]1[O:8][C@H:7]([CH2:9][OH:10])[C@@H:6]([OH:11])[C@H:5]([OH:12])[C@H:4]1[OH:13].[Cl:14][C:15]1[C:20]([OH:21])=[C:19]([Cl:22])[C:18]([Cl:23])=[C:17]([Cl:24])[C:16]=1[Cl:25].[Al].[CH2:27]([O:29][P:30]([O:34][CH2:35][CH3:36])[O:31][CH2:32][CH3:33])[CH3:28].[CH2:37]1[O:40][CH:38]1[CH3:39]>[Fe].C(N(CC)CC)C>[CH3:1][O:2][C@H:3]1[O:8][C@H:7]([CH2:9][OH:10])[C@@H:6]([OH:11])[C@H:5]([OH:12])[C@H:4]1[OH:13].[CH2:27]([O:29][P:30]([O:34][CH2:35][CH3:36])[O:31][CH2:32][CH3:33])[CH3:28].[Cl:14][C:15]1[C:20]([OH:21])=[C:19]([Cl:22])[C:18]([Cl:23])=[C:17]([Cl:24])[C:16]=1[Cl:25].[CH2:37]1[O:40][CH:38]1[CH3:39]

参加物

8

反応物 5

HCID 992PentachlorophenolHCID 6378Propylene Oxide2 回HCID 31215Triethyl phosphiteHCID 64947methyl alpha-D-glucopyranosideHCID 5359268Aluminum

生成物 1

HCID 131710245HCID 131710245、化合物

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 8471Triethylamine溶媒

反応条件

温度
122 °C

実験手順

A 5-liter flask, standardly equipped, was charged with 776 grams of alpha-methylglucoside, 1264 grams of pentachlorophenol containing about 750 ppm of aluminum and iron compounds, 240 grams of triethylphosphite, and heated to 122°C. 1025 ml. of propylene oxide was added at 122°-138°C. over a 6-hour period. Then 48 grams of triethylamine was added, followed by 265 ml. more of propylene oxide to reduce the acid number to less than 1. The mixture was then stripped for 2 hours at 80°-85°C/2 mm. Hg to remove volatiles. The oxypropylated product weighed 3827 grams and analyzed as follows:

後処理

  1. customA 5-liter flask, standardly equipped
  2. custom/2 mm. Hg to remove volatiles

出典と根拠

ORDレコード
ord-5023106919ff4622976632ee697b3ffb
出典データセット
uspto-grants-1976_05
特許番号
US03957922

反応ノート

読み込み中…