Chlorotrimethylsilane → D-2-Aminohexano-6-lactam

反応式

Cl.[NH2:2][C@@H:3]([C:9]([OH:11])=O)[CH2:4][CH2:5][CH2:6][CH2:7][NH2:8].C[Si](C)(C)N[Si](C)(C)C.Cl[Si](C)(C)C>C1(C)C(C)=CC=CC=1>[NH2:2][C@@H:3]1[CH2:4][CH2:5][CH2:6][CH2:7][NH:8][C:9]1=[O:11]

参加物

反応条件

温度: 120 °C

実験手順

To a solution of (R)-lysine HCl salt (100 g, 0.68 mol) in xylene (1 L) was added hexamethyldisilazane (1000 mL, 4.76 mol) and chlorotrimethylsilane (10 mL, 78.8 mmol). The mixture was heated to 120° C. for 24 h, then to 180° C. for 48 h. The solvent was then removed under reduced pressure and the crude material was purified by column chromatography (20:1 to 10:1 CH2Cl2/MeOH) to afford (R)-3-aminoazepan-2-one (I-1a).

後処理

customThe solvent was then removed under reduced pressure
customthe crude material was purified by column chromatography (20:1 to 10:1 CH2Cl2/MeOH)

出典と根拠

ORDレコード: ord-6d4b5949406f44f498638a066d6521b7
出典データセット: uspto-grants-2016_09
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09440957B2

反応ノート

読み込み中…

参加物

反応物 3

HCID 6397Chlorotrimethylsilane

HCID 13838Hexamethyldisilazane

HCID 81691Lysine hydrochloride, D-

生成物 1

HCID 439823D-2-Aminohexano-6-lactam

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

反応条件

温度: 120 °C

実験手順

後処理

customThe solvent was then removed under reduced pressure
customthe crude material was purified by column chromatography (20:1 to 10:1 CH2Cl2/MeOH)

出典と根拠

ORDレコード: ord-6d4b5949406f44f498638a066d6521b7
出典データセット: uspto-grants-2016_09
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US09440957B2

反応ノート

読み込み中…