Thionyl Chloride → HCID 54316934、化合物

HRID 1415432ノート

反応式

HRID 1415432 の反応式
[O:1]=[C:2]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:14][CH2:15][C:16]([OH:18])=O.S(Cl)([Cl:21])=O>C1C=CC=CC=1>[O:1]=[C:2]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH:3]1[CH2:14][CH2:15][C:16]([Cl:21])=[O:18]

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 27750833-(2-oxocyclododecyl)propanoic acid

生成物 1

HCID 54316934HCID 54316934、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

Ten parts of β-(2-oxocyclododecyl)propionic acid, 6 parts of thionyl chloride, and 35 parts of anhydrous benzene were placed into a reactor and allowed to stand at 0° C for 3 hours and further at room temperature overnight. Then, the excess amount of thionyl chloride and the benzene were distilled off under reduced pressure to give β-(2-oxocyclododecyl)propionic acid chloride. The acid chloride was dissolved in 25 parts of benzene. Into the resulting solution was added dropwise 35 parts of benzene solution containing 30 wt.% pyridine and the mixture was stirred for 6 hours. The produced crystals were filtered off. The filtrate was washed with dilute hydrochloric acid to remove excess pyridine, the organic layer was washed to remove the hydrochloric acid, and then dried with Glauber's salt. Thereafter the resulting solution was treated by the same method as in Example 1 to give 6.3 parts of 13-oxabicyclo(10.4.0)-hexadec-1(12)-en-14-one in 68.4% yield.

後処理

  1. distillationThen, the excess amount of thionyl chloride and the benzene were distilled off under reduced pressure

出典と根拠

ORDレコード
ord-873106bb22714aaabe4e7099473b4f51
出典データセット
uspto-grants-1977_01
特許番号
US04005107

反応ノート

読み込み中…