Triphenylphosphine → HCID 20139063, compound

HRID 978359Notes

Reaction equation

[Br:1][CH2:2][C:3]1[C:8]2[C:9](=[O:16])[O:10][C:11]([O:13][CH2:14][CH3:15])=[N:12][C:7]=2[CH:6]=[CH:5][CH:4]=1.[C:17]1([P:23]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C1(C)C=CC=CC=1>[Br-:1].[CH2:14]([O:13][C:11]1[O:10][C:9](=[O:16])[C:8]2[C:3]([CH2:2][P+:23]([C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)([C:30]3[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=3)[C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)=[CH:4][CH:5]=[CH:6][C:7]=2[N:12]=1)[CH3:15]

Participants

Conditions

Temperature: 60 °C

Procedure

A solution of 5-bromomethyl-2-ethoxy-4H-3,1-benzoxazin-4-one (3.15 gm), prepared as described in Example VI above, and triphenylphosphine (5.44 gm) in toluene was heated at 60° C. for 6 hours. The insoluble precipitate was filtered, and the mother liquor was reduced to half of its original volume and refiltered, yielding 9 gm of 1-(2-ethoxy-4H-3,1-benzoxazin-4-on-5-yl)-methyl-triphenylphosphonium bromide, m.p. (turns yellow at) 125° C. IR: 1740, 1640 cm-1 ;, decom. 135°-140° C.

Workup

filtrationThe insoluble precipitate was filtered

Sources & evidence

ORD record: ord-729b77ccb3cc4bc7add14e2ad7544e00
Source dataset: uspto-grants-1987_05
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US04665070

Reaction notes

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