Triethylamine → tert-butyl N-(2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepin-3-yl)carbamate

HRID 482748노트

반응식

HRID 482748 반응식
[NH2:1][CH:2]1[CH2:8][CH2:7][C:6]2[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=2[NH:4][C:3]1=[O:13].[C:14]([O:18][C:19](ON=C(C1C=CC=CC=1)C#N)=[O:20])([CH3:17])([CH3:16])[CH3:15].C(N(CC)CC)C>O.O1CCOCC1>[C:14]([O:18][C:19]([NH:1][CH:2]1[CH2:8][CH2:7][C:6]2[CH:9]=[CH:10][CH:11]=[CH:12][C:5]=2[NH:4][C:3]1=[O:13])=[O:20])([CH3:17])([CH3:16])[CH3:15]

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 938652-(tert-Butoxycarbonyloxyimino)-2-phenylacetonitrileHCID 44344333-Amino-2,3,4,5-tetrahydro-1H-benzazepin-2-one

생성물 1

HCID 13243501tert-butyl N-(2-oxo-2,3,4,5-tetrahydro-1H-1-benzazepin-3-yl)carbamate

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

A solution of 3-amino-2,3,4,5-tetrahydro-1H[1]benzazepin-2-one (4.0 g), 2-t-butyloxycarbonyloxyimino-2-phenylacetonitrile (6.1 g) and triethylamine (5 ml) in water (20 ml) and dioxane (25 ml) was stirred at room temperature for 18 hours. The resulting solid was filtered off and washed with water. Recrystallization from ethyl acetate gave 3-t-butyloxycarbonylamino-2,3,4,5-tetrahydro-1H-[1]benzazepin-2-one, m.p. 199°-201°.

후처리

  1. filtrationThe resulting solid was filtered off
  2. washwashed with water
  3. customRecrystallization from ethyl acetate

출처 및 근거

ORD 기록
ord-d2b0010bc2bf4f41acf908b3335decb9
출처 데이터셋
uspto-grants-1986_03
특허 번호
US04575503

반응 노트

불러오는 중…