Triethylamine → Tert-butyl 1-(aminoimino-methyl)-piperidin-4-ylmethylcarbamate hemisulfite

HRID 963853

反応式

HRID 963853 の反応式
[NH:1]1[CH2:6][CH2:5][CH:4]([CH2:7][NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH2:3][CH2:2]1.C([N:18]([CH2:21]C)CC)C.[C:23]([S:26]([OH:29])(=[O:28])=[O:27])([NH2:25])=[NH:24]>CN(C=O)C>[S:26]([OH:29])([OH:28])=[O:27].[NH2:24][N:18]=[CH:21][N:1]1[CH2:6][CH2:5][CH:4]([CH2:7][NH:8][C:9](=[O:15])[O:10][C:11]([CH3:12])([CH3:14])[CH3:13])[CH2:3][CH2:2]1.[C:11]([O:10][C:9](=[O:15])[NH:8][CH2:7][CH:4]1[CH2:5][CH2:6][N:1]([CH:23]=[N:25][NH2:18])[CH2:2][CH2:3]1)([CH3:12])([CH3:14])[CH3:13]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 723429Tert-butyl (piperidin-4-ylmethyl)carbamateHCID 9877361Methanesulfonic acid, aminoimino-

生成物 1

HCID 131720709Tert-butyl 1-(aminoimino-methyl)-piperidin-4-ylmethylcarbamate hemisulfite

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 130 g of 1,1-dimethylethyl (4piperidinylmethyl)-carbamate in 1300 ml of DMF is treated with 138 ml of triethylamine and 61.8 g of formamidinesulfonic acid and the mixture is stirred at room temperature overnight. The precipitated material is filtered, suspended in 500 ml of ethanol, again filtered off and dried. There are obtained 65.6 g of tert-butyl 1-(aminoimino-methyl)-piperidin-4-ylmethylcarbamate hemisulfite, MS (ISP): 257.4 (M+H)+.

後処理

  1. filtrationThe precipitated material is filtered
  2. filtrationagain filtered off
  3. customdried

出典と根拠

ORDレコード
ord-86e6069001dc41e4af4476953984ac18
出典データセット
uspto-grants-1998_06
特許番号
US05763604

関連ノート

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