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Diisopropylethylamine → 1009368-28-8

HRID 1051163
ノート
印刷プレビュー

反応式

HRID 1051163 の反応式
[OH:1][CH:2]1[CH2:5][N:4]([C:6]([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7])[CH2:3]1.CCN(C(C)C)C(C)C.[Cl:22][C:23](Cl)([O:25]C(=O)OC(Cl)(Cl)Cl)Cl>C1COCC1>[Cl:22][C:23]([O:1][CH:2]1[CH2:3][N:4]([C:6]([O:8][C:9]([CH3:12])([CH3:11])[CH3:10])=[O:7])[CH2:5]1)=[O:25]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 94429TriphosgeneHCID 2756801Tert-butyl 3-hydroxyazetidine-1-carboxylate

生成物 1

HCID 576866831009368-28-8収率 55%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of 3-hydroxy-1-Boc azetidine (21; 350 mg, 2.023 mmol) and DIPEA (1.3 ml, 7.080 mmol) in THF (5 ml) at 0° C. was slowly added triphosgene (898 mg, 3.034 mmol). The resulting mixture was stirred for 2 hr at RT. After completion of the reaction, the reaction mixture was filtered and washed with fresh THF to get rid of inorganic salts. The filtrate was concentrated under reduced pressure to get crude product 61 in 55% yield. The crude product, thus obtained, was immediately used for the next reaction.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. customat 0° C.
  2. customAfter completion of the reaction
  3. filtrationthe reaction mixture was filtered
  4. washwashed with fresh THF
  5. customto get rid of inorganic salts
  6. concentrationThe filtrate was concentrated under reduced pressure
  7. customto get crude product 61 in 55% yield

出典と根拠

ORDレコード
ord-f0f4ee96e03d4824a54279b02f13644e
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09388164B2

反応ノート

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