Hydrochloric Acid → HCID 54335685、化合物

反応式

[O:1]=[C:2]([C:7]([CH3:10])([CH3:9])[CH3:8])[C:3]([NH:5][CH3:6])=[O:4].Cl>CO.C(Cl)Cl>[OH:1][C@@H:2]([C:7]([CH3:10])([CH3:9])[CH3:8])[C:3]([NH:5][CH3:6])=[O:4]

参加物

実験手順

The experiment was carried out in an analogous manner to Example 1. The asymmetric hydrogenation of 55.0 g (0.384 mol) of 2-keto-3,3,N-trimethyl-butyramide in 270 ml of methanol and 30 ml of methylene chloride in the presence of a catalyst prepared from 296 mg (0.384 mmol) of [Ru(OAc)2((S)-BIPHEMP)] and 31 ml of a 0.025 molar methanolic hydrochloric acid solution gave, after crystallization, 34.4 g (62%) of (S)-2-hydroxy-3,3,N-trimethyl-butyramide, m.p.=60-62° C., [α]=−59.9° (c=1, CHCl3), ee=99.2%.

後処理

customgave
customafter crystallization, 34.4 g (62%) of (S)-2-hydroxy-3,3,N-trimethyl-butyramide, m.p.=60-62° C., [α]=−59.9° (c=1, CHCl3), ee=99.2%

出典と根拠

ORDレコード: ord-15a7b538dd284072a1e8b046786d3c00
出典データセット: uspto-grants-2002_02
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US06348612B1

反応ノート

読み込み中…

参加物

反応物 2

HCID 313Hydrochloric Acid

HCID 13355140HCID 13355140、化合物

生成物 1

HCID 54335685HCID 54335685、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒

HCID 6344Dichloromethane溶媒

実験手順

後処理

customgave
customafter crystallization, 34.4 g (62%) of (S)-2-hydroxy-3,3,N-trimethyl-butyramide, m.p.=60-62° C., [α]=−59.9° (c=1, CHCl3), ee=99.2%

出典と根拠

ORDレコード: ord-15a7b538dd284072a1e8b046786d3c00
出典データセット: uspto-grants-2002_02
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US06348612B1

反応ノート

読み込み中…