Ethanesulfonic acid → HCID 12764425, compound

HRID 1155094Notes

Reaction equation

HRID 1155094 reaction equation
[CH2:1]([S:3]([OH:6])(=[O:5])=[O:4])[CH3:2].[CH:7]1([CH2:10][N:11]2[CH:18]3[CH2:19][N:14]([C:15]4[CH:23]=[C:22]([NH2:24])[CH:21]=[CH:20][C:16]=4[CH2:17]3)[CH2:13][CH2:12]2)[CH2:9][CH2:8]1>C(O)(C)C.CO>[CH2:1]([S:3]([OH:6])(=[O:5])=[O:4])[CH3:2].[CH2:1]([S:3]([OH:6])(=[O:5])=[O:4])[CH3:2].[CH:7]1([CH2:10][N:11]2[CH:18]3[CH2:19][N:14]([C:15]4[CH:23]=[C:22]([NH2:24])[CH:21]=[CH:20][C:16]=4[CH2:17]3)[CH2:13][CH2:12]2)[CH2:8][CH2:9]1

Participants

5

Reactant 2

HCID 11668Ethanesulfonic acidHCID 1335394-(Cyclopropylmethyl)-3,4,5,6-tetrahydro-2H-1,5-methano-1,4-benzodiazocin-9-amine

Product 1

HCID 12764425HCID 12764425, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 3776IsopropanolSolvent

Procedure

A solution of ethanesulfonic acid (24 g.) in isopropyl alcohol (80 ml.) was added with warming (40°-50° C.) to a solution of 4-cyclopropylmethyl-9-amino-3,4,5,6-tetrahydro-2H-1,5-methano-1,4-benzodiazocine (26.9 g.) in methanol (120 ml.), affording 4-cyclopropylmethyl-9-amino-3,4,5,6-tetrahydro-2H-1,5-methano-1,4-benzodiazocine diethanesulfonate in two crops (34 g., m.r. 221-225° C.; 14 g., m.r. 211°-219° C.), the second of which was recrystallized from methanol-isopropyl alcohol (10 g., m.r. 221°-224° C.).

Sources & evidence

ORD record
ord-896cee19cb0944538be7ba712b2c50a1
Source dataset
uspto-grants-1981_11
Patent number
US04299830

Reaction notes

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