Hydrochloric Acid → HCID 58380880、化合物

HRID 1948159ノート

反応式

HRID 1948159 の反応式
[CH3:1][O:2][N:3]([CH3:12])[C:4](=[O:11])[C:5]([C:7]([F:10])([F:9])[F:8])=[CH2:6].C[Si](C)(C)[O:15][C:16]([CH:18]=[CH2:19])=[CH2:17].Cl>C1COCC1>[CH3:1][O:2][N:3]([CH3:12])[C:4]([C:5]1([C:7]([F:10])([F:8])[F:9])[CH2:19][CH2:18][C:16](=[O:15])[CH2:17][CH2:6]1)=[O:11]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 5546572-(Trimethylsiloxy)-1,3-butadieneHCID 114580682-Propenamide, N-methoxy-N-methyl-2-(trifluoromethyl)-

生成物 1

HCID 58380880HCID 58380880、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

21.8 g (119 mmol) of N-Methoxy-N-methyl-2-trifluoromethyl-acrylamide (67) and 36.1 ml (29.6 mmol) of 2-(trimethylsiloxy)-1,3-butadiene were mixed and divided into 3 portions. Each portion was treated at 120° C. under microwave irradiation for 2 h. The combined reaction products were then diluted using 150 ml of THF, 100 ml of a 5% aqueous solution of HCl was added and stirred for 1 h at ambient temperature. Afterwards, the mixture was extracted three times using 200 ml of ethyl acetate each, dried using MgSOt and evaporated to yield 18.0 g, used without further purification. Rt=0.72 min (Method P).

後処理

  1. additionEach portion was treated at 120° C. under microwave irradiation for 2 h
  2. customThe combined reaction products
  3. additionwere then diluted
  4. additionwas added
  5. extractionAfterwards, the mixture was extracted three times
  6. customdried
  7. customevaporated
  8. customto yield 18.0 g
  9. customused without further purification

出典と根拠

ORDレコード
ord-c3c6b04c9592419b8801d03943793262
出典データセット
uspto-grants-2013_03
特許番号
US08399482B2

反応ノート

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