홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Triethylamine → HCID 54374598, 화합물

HRID 2412858
노트
인쇄 미리보기

반응식

HRID 2412858 반응식
C(O)(=O)C.[C:5]([C:7](=[N:11][O:12][CH2:13][C:14]([O:16][CH3:17])=[O:15])[C:8]([NH2:10])=[NH:9])#[N:6].C(N(CC)CC)C.BrBr.[S-:27][C:28]#[N:29].[K+]>CO>[CH3:17][O:16][C:14]([CH2:13][O:12][N:11]=[C:7]([C:8]1[N:10]=[C:28]([NH2:29])[S:27][N:9]=1)[C:5]#[N:6])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 24408BromineHCID 516872Potassium thiocyanateHCID 86739873HCID 86739873, 화합물

생성물 1

HCID 54374598HCID 54374598, 화합물수율 87.9%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To a suspension of 2-cyano-2-methoxycarbonylmethoxyiminoacetamidine acetate (495 g) in methanol (4.95 l) was dropped triethylamine (512.6 g) at -10° C. under stirring and cooling, and further, bromine (357.3 g) was added to the above mixture at the same temperature. After the reaction mixture was stirred for 15 minutes, a solution of potassium thiocyanate (216 g) in methanol (2.16 l) was dropped thereto at -10° to -5° C. under stirring, which was continued for 30 minutes at 0° to 5° C. The resulting precipitates were collected by filtration, washed with water (5 l) and dried to give 2-methoxycarbonylmethoxyimino-2-(5-amino-1,2,4-thiadiazol-3-yl)acetonitrile (syn isomer) (430 g), which was recrystallized from aqueous methanol, mp. 225° to 227° C. (dec.).

후처리

  1. temperaturecooling
  2. stirringAfter the reaction mixture was stirred for 15 minutes
  3. stirringat -10° to -5° C. under stirring
  4. customThe resulting precipitates
  5. filtrationwere collected by filtration
  6. washwashed with water (5 l)
  7. customdried

출처 및 근거

ORD 기록
ord-116b926eb9c64945bb5908981d8b11f9
출처 데이터셋
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04495182

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트