Thionyl Chloride → HCID 54316934, 화합물

HRID 1415432노트

반응식

HRID 1415432 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 54316934HCID 54316934, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-873106bb22714aaabe4e7099473b4f51
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04005107

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