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

HRID 963853

반응식

HRID 963853 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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)+.

후처리

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

출처 및 근거

ORD 기록
ord-86e6069001dc41e4af4476953984ac18
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05763604

연결된 노트

불러오는 중…