Methyldichlorosilane → HCID 11814019, compound

HRID 2392935Notes

Reaction equation

[CH3:1][N:2]([CH3:44])[C:3]1[CH:8]=[CH:7][C:6]([P:9]([C:35]2[CH:40]=[CH:39][C:38]([N:41]([CH3:43])[CH3:42])=[CH:37][CH:36]=2)([CH2:11][CH2:12][CH2:13][CH2:14][P:15]([C:26]2[CH:31]=[CH:30][C:29]([N:32]([CH3:34])[CH3:33])=[CH:28][CH:27]=2)([C:17]2[CH:22]=[CH:21][C:20]([N:23]([CH3:25])[CH3:24])=[CH:19][CH:18]=2)=O)=O)=[CH:5][CH:4]=1.C(N(CCCC)CCCC)CCC.C[SiH](Cl)Cl>CC1C=CC=CC=1C>[CH3:34][N:32]([CH3:33])[C:29]1[CH:30]=[CH:31][C:26]([P:15]([C:17]2[CH:18]=[CH:19][C:20]([N:23]([CH3:24])[CH3:25])=[CH:21][CH:22]=2)[CH2:14][CH2:13][CH2:12][CH2:11][P:9]([C:6]2[CH:7]=[CH:8][C:3]([N:2]([CH3:1])[CH3:44])=[CH:4][CH:5]=2)[C:35]2[CH:40]=[CH:39][C:38]([N:41]([CH3:42])[CH3:43])=[CH:37][CH:36]=2)=[CH:27][CH:28]=1

Participants

Conditions

Temperature: 50 °C

Procedure

6.1 g (10 mmol) of 1,4-bis[bis(4-dimethylaminophenyl)phosphinyl]butane and 9.3 g (50 mmol) of tri-n-butylamine are initially charged in 30 ml of o-xylene in an argon atmosphere. 5.75 g (50 mmol) of methyldichlorosilane are slowly added dropwise with the reaction mixture warming up to 50° C. It is subsequently heated to 100° C. and stirred for 4 hours, then heated to 145° C. and stirred for 16 hours. Cooling the clear solution results in formation of colorless crystals which are filtered off and washed with 10 ml of degassed o-xylene. Drying in a high vacuum gives 5.5 g of colorless crystals, corresponding to a yield of 95%.

Workup

temperatureIt is subsequently heated to 100° C.
temperatureheated to 145° C.
stirringstirred for 16 hours
temperatureCooling the clear solution
customresults in formation of colorless crystals which
filtrationare filtered off
washwashed with 10 ml of degassed o-xylene
customDrying in a high vacuum

Sources & evidence

ORD record: ord-7fb7413666bf49c1bba410be0e0e0cca
Source dataset: uspto-grants-1998_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US05801287

Reaction notes

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