Dichloromethane → HCID 66895991, compound

HRID 1511572Notes

Reaction equation

HRID 1511572 reaction equation
[CH:1]1([S:4]([NH:7][C:8]([C@@:10]2([NH:15]C(=O)OC(C)(C)C)[CH2:12][C@H:11]2[CH2:13][CH3:14])=[O:9])(=[O:6])=[O:5])[CH2:3][CH2:2]1.C(Cl)[Cl:24]>>[ClH:24].[NH2:15][C@:10]1([C:8]([NH:7][S:4]([CH:1]2[CH2:3][CH2:2]2)(=[O:6])=[O:5])=[O:9])[CH2:12][C@H:11]1[CH2:13][CH3:14]

Participants

3

Reactant 2

HCID 6344DichloromethaneHCID 70324238HCID 70324238, compound

Product 1

HCID 66895991HCID 66895991, compound

Procedure

A solution of the product from Step 1 above (92 g, 0.28 mol) in DCM (1200 mL) was cooled to 0° C. and HCl bubbled through the solution for 10 min, the cooling bath removed and the reaction mixture stirred for 2 h. Nitrogen was bubbled through the reaction mixture for 5 min and the volatiles evaporated. The residue was azeotroped with DCM (×3) to give an off white powder (75 g).

Workup

  1. customHCl bubbled through the solution for 10 min
  2. customthe cooling bath removed
  3. customNitrogen was bubbled through the reaction mixture for 5 min
  4. customthe volatiles evaporated
  5. customThe residue was azeotroped with DCM (×3)

Sources & evidence

ORD record
ord-d7c0a9c8b0ad47aa8ab2bfb64ab500e8
Source dataset
uspto-grants-2012_07
Patent number
US08216999B2

Reaction notes

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