Diisopropylethylamine → HCID 69507675、化合物

HRID 1374553ノート

反応式

HRID 1374553 の反応式
O[C:2]1C2N=NNC=2C=CC=1.C(N(C(C)C)CC)(C)C.Cl.CN(C)CCCN=C=NCC.[NH2:32][C@@H:33]1[C:39](=[O:40])[N:38]([CH:41]2[CH2:43][CH2:42]2)[C:37]2[CH:44]=[CH:45][CH:46]=[CH:47][C:36]=2[N:35]([CH3:48])[CH2:34]1.[C:49]([OH:54])(=O)[C@H:50]([CH3:52])[OH:51]>C1COCC1>[CH:43]1([CH2:41][N:38]2[C:39](=[O:40])[C@@H:33]([NH:32][C:49](=[O:54])[C@@H:50]([OH:51])[CH3:52])[CH2:34][N:35]([CH3:48])[C:36]3[CH:47]=[CH:46][CH:45]=[CH:44][C:37]2=3)[CH2:42][CH2:2]1

参加物

7

反応物 5

HCID 81531DiisopropylethylamineHCID 107689L-Lactic AcidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 69507494HCID 69507494、化合物HCID 178418300HCID 178418300、化合物

生成物 1

HCID 69507675HCID 69507675、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Hydroxybenzotriazole (121 mg, 1 mmol), diisopropylethylamine (23 2 mg, 2 mmol) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (172 mg, 1 mmol) were added to a cooled (0° C.) solution of (S)-3-amino-1-cyclopropyl-5-methyl-1,3,4,5-tetrahydro-benzo[b][1,4]diazepin-2-one (220 mg, 1 mmol) and L-(+)-lactic acid (81 mg, 1 mmol) in THF (2 ml) and stirred overnight at r.t. The solvent was evaporated, the residue was taken up in dichloromethane and washed with water. The organic phase was dried over Na2SO4 and evaporated. Upon chromatographic purification (silica gel, dichloromethane/methanol=1:0−9:1) the title compound (347 mg, quant.) was obtained as a white solid.

後処理

  1. customThe solvent was evaporated
  2. washwashed with water
  3. dry with materialThe organic phase was dried over Na2SO4
  4. customevaporated
  5. customUpon chromatographic purification (silica gel, dichloromethane/methanol=1:0−9:1) the title compound (347 mg, quant.)
  6. customwas obtained as a white solid

出典と根拠

ORDレコード
ord-cc22f71021d94a0cbed3c6cbbbe8695b
出典データセット
uspto-grants-2007_01
特許番号
US07166587B2

反応ノート

読み込み中…