Dichloromethane → HCID 66895991, compound

HRID 2045690Notes

Reaction equation

HRID 2045690 reaction equation
C(OC(=O)[NH:7][C@:8]1([C:13]([NH:15][S:16]([CH:19]2[CH2:21][CH2:20]2)(=[O:18])=[O:17])=[O:14])[CH2:10][C@H:9]1[CH2:11][CH3:12])(C)(C)C.C(Cl)[Cl:24]>>[ClH:24].[NH2:7][C@:8]1([C:13]([NH:15][S:16]([CH:19]2[CH2:21][CH2:20]2)(=[O:18])=[O:17])=[O:14])[CH2:10][C@H:9]1[CH2:11][CH3:12]

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 was bubbled through the solution. After 10 min, the cooling bath was removed, and the reaction mixture was 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). LRMS (M+H)+ Calcd.=233; found 233.

Workup

  1. customHCl was bubbled through the solution
  2. customthe cooling bath was 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-4bc9a5c7dd95427e9ddca8c39b547a47
Source dataset
uspto-grants-2013_11
Patent number
US08591878B2

Reaction notes

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