Water → HCID 136024931, compound

HRID 2395255Notes

Reaction equation

HRID 2395255 reaction equation
[OH:1][C:2]1[C:7]([C:8]([CH3:11])([CH3:10])[CH3:9])=[CH:6][C:5]([C:12]2[CH:16]=[C:15]([CH:17]=[CH:18][P:19](=[O:26])([O:23]CC)[O:20]CC)[O:14][N:13]=2)=[CH:4][C:3]=1[C:27]([CH3:30])([CH3:29])[CH3:28].C[Si](C)(C)Br.O>ClCCl>[OH:1][C:2]1[C:3]([C:27]([CH3:30])([CH3:29])[CH3:28])=[CH:4][C:5]([C:12]2[CH:16]=[C:15]([CH:17]=[CH:18][P:19](=[O:20])([OH:23])[OH:26])[O:14][N:13]=2)=[CH:6][C:7]=1[C:8]([CH3:11])([CH3:10])[CH3:9]

Participants

5

Procedure

4.0 g (0.009 mol) of the product from Example 57 were stirred, under a protective gas and at room temperature, in 300 ml of absolute dichloromethane together with 3.9 ml (0.03 mol) of trimethylbromosilane until the reaction was complete (monitoring by TLC). After adding 0.5 ml of water, the mixture was concentrated; the residue was taken up several times in methanol and concentrated under reduced pressure. The oil was stirred with tert-butyl methyl ether until a crystalline residue remained. Yield: 3.0 g.

Workup

  1. concentrationthe mixture was concentrated
  2. concentrationconcentrated under reduced pressure

Sources & evidence

ORD record
ord-c89990c140e341adaa450ea0f8fb1da4
Source dataset
uspto-grants-1998_09
Patent number
US05814627

Reaction notes

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