Trimethyl orthoformate → 5-({[3-Iodo-4-(methoxy)phenyl]amino}methylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione

HRID 1042979

반응식

HRID 1042979 반응식
[CH3:1][C:2]1([CH3:10])[O:7][C:6](=[O:8])[CH2:5][C:4](=[O:9])[O:3]1.[CH3:11]OC(OC)OC.[I:18][C:19]1[CH:20]=[C:21]([CH:23]=[CH:24][C:25]=1[O:26][CH3:27])[NH2:22]>>[I:18][C:19]1[CH:20]=[C:21]([NH:22][CH:11]=[C:5]2[C:6](=[O:8])[O:7][C:2]([CH3:10])([CH3:1])[O:3][C:4]2=[O:9])[CH:23]=[CH:24][C:25]=1[O:26][CH3:27]

참가 물질

4

반응물 3

HCID 9005Trimethyl orthoformateHCID 162492,2-Dimethyl-1,3-dioxane-4,6-dioneHCID 220545963-Iodo-4-methoxyaniline

생성물 1

HCID 574655765-({[3-Iodo-4-(methoxy)phenyl]amino}methylidene)-2,2-dimethyl-1,3-dioxane-4,6-dione수율 85.9%

실험 절차

A mixture of 2,2-dimethyl-1,3-dioxane-4,6-dione (203 g, 1.4 mol) and trimethoxymethane (1.51) was heated to reflux for 1 h, then the 3-iodo-4-methoxy-aniline (349.2 g, 1.402mol) was added portionwise. The reaction mixture was stirred at reflux for 1 h, then cooled to room temperature. The resulting precipitate was filtered off, washed with diisopropyl ether and dried to give the title compound as a beige powder (485 g, 85.9%)

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 1 h
  3. temperatureat reflux for 1 h
  4. filtrationThe resulting precipitate was filtered off
  5. washwashed with diisopropyl ether
  6. customdried

출처 및 근거

ORD 기록
ord-b651989284a04411be9a123ed9508a84
출처 데이터셋
uspto-grants-2013_10
특허 번호
US08557984B2

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