Hydrochloric Acid → HCID 12961947, compound

HRID 1065691Notes

Reaction equation

HRID 1065691 reaction equation
[ClH:1].[C:2]([O:5][C@H:6]1[CH2:23][CH2:22][C@@:21]2([CH3:24])[C@@H:8]([CH2:9][CH2:10][C@@H:11]3[C@@H:20]2[CH2:19][CH2:18][C@@:16]2([CH3:17])[C@H:12]3[CH2:13][C@@H:14]([OH:27])[C@@H:15]2[NH:25][CH3:26])[CH2:7]1)(=[O:4])[CH3:3].CCOCC>CO.C(Cl)(Cl)Cl>[ClH:1].[C:2]([O:5][C@H:6]1[CH2:23][CH2:22][C@@:21]2([CH3:24])[C@@H:8]([CH2:9][CH2:10][C@@H:11]3[C@@H:20]2[CH2:19][CH2:18][C@@:16]2([CH3:17])[C@H:12]3[CH2:13][C@@H:14]([OH:27])[C@@H:15]2[NH:25][CH3:26])[CH2:7]1)(=[O:4])[CH3:3]

Participants

6

Reactant 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 12961946HCID 12961946, compound

Product 1

HCID 12961947HCID 12961947, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolvent2×HCID 6212ChloroformSolvent

Procedure

A cold (0° C.) solution of hydrogen chloride (2 g) in methanol (10 ml) was added with stirring to a solution of 17β-methylamino-5α-androstane-3β,16α-diol 3-acetate (16 g) in methanol (16 ml) and chloroform (48 ml) at 0° C. Ether (300 ml) was added to precipitate 17β-methylamino-5α-androstane-3β,16α-diol 3-acetate hydrochloride as prisms (16 g), m.p. >270° C. (decomp.), [α]D +113° (C 1.04 in MeOH).

Workup

  1. customto precipitate 17β-methylamino-5α-androstane-3β,16α-diol 3-acetate hydrochloride as prisms (16 g), m.p. >270° C. (decomp.), [α]D +113° (C 1.04 in MeOH)

Sources & evidence

ORD record
ord-bec4db4888754b1eb77e20a5cfd7951f
Source dataset
uspto-grants-1982_05
Patent number
US04330539

Reaction notes

Loading…