Water → tert-Butyl 5-(2-trifluoromethylbenzoyl)-3,4,5,6-tetrahydro-1H-pyrrolo[3,4-c]pyrrole-2-carboxylate

HRID 1186775ノート

反応式

HRID 1186775 の反応式
Cl.[CH2:2]1[C:6]2[CH2:7][NH:8][CH2:9][C:5]=2[CH2:4][N:3]1[C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11].C(N(CC)CC)C.[F:24][C:25]([F:36])([F:35])[C:26]1[CH:34]=[CH:33][CH:32]=[CH:31][C:27]=1[C:28](Cl)=[O:29].O>C(Cl)Cl>[F:24][C:25]([F:35])([F:36])[C:26]1[CH:34]=[CH:33][CH:32]=[CH:31][C:27]=1[C:28]([N:8]1[CH2:7][C:6]2[CH2:2][N:3]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:4][C:5]=2[CH2:9]1)=[O:29]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 675612-(Trifluoromethyl)benzoyl chlorideHCID 45792433tert-butyl 1H,2H,3H,4H,5H,6H-pyrrolo(3,4-c)pyrrole-2-carboxylate hydrochloride

生成物 1

HCID 58075189tert-Butyl 5-(2-trifluoromethylbenzoyl)-3,4,5,6-tetrahydro-1H-pyrrolo[3,4-c]pyrrole-2-carboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

tert-Butyl 3,4,5,6-tetrahydro-1H-pyrrolo[3,4-C]pyrrole-2-carboxylate hydrochloride (30 g, 121.6 mmol) was suspended in 700 ml of methylene chloride, triethylamine (50.7 ml, 364.8 mmol) was added with ice bath cooling, and 2-(trifluoromethyl)benzoyl chloride (25.22 ml, 171.2 mmol) was slowly added dropwise. The brown suspension was stirred for 2 h, in the course of which it was allowed to come to RT. The reaction mixture was admixed with water, and the organic phase was removed, dried and concentrated by rotary evaporation. The crude product (56.8 g) was converted further without purification.

後処理

  1. temperaturecooling
  2. customto come to RT
  3. customthe organic phase was removed
  4. customdried
  5. concentrationconcentrated by rotary evaporation
  6. customThe crude product (56.8 g) was converted further without purification

出典と根拠

ORDレコード
ord-c8919835bd52435098e98114a3b10906
出典データセット
uspto-grants-2014_03
特許番号
US08673917B2

反応ノート

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